data_dm-aj-53_mo_sq
_audit_creation_date              2018-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_publ_contact_author_address      ?
_publ_contact_author_email        ?
_publ_contact_author_id_orcid     ?
_publ_contact_author_name         ''
_publ_contact_author_phone        ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
;
_chemical_name_common             ?
_chemical_name_systematic         ?
_chemical_formula_moiety          '0.4(C23 N3 O Pd)'
_chemical_formula_sum             'C9.20 N1.20 O0.40 Pd0.40'
_chemical_formula_weight          176.26
_chemical_melting_point           ?
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pd' 'Pd' -0.9988 1.0072
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system       'triclinic'
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                    9.6348(3)
_cell_length_b                    10.7198(3)
_cell_length_c                    11.5837(3)
_cell_angle_alpha                 105.639(2)
_cell_angle_beta                  103.125(2)
_cell_angle_gamma                 104.695(3)
_cell_volume                      1056.87(6)
_cell_formula_units_Z             5
_cell_measurement_reflns_used     8947
_cell_measurement_temperature     150
_cell_measurement_theta_max       31.2560
_cell_measurement_theta_min       2.2880
_shelx_estimated_absorpt_T_max    ?
_shelx_estimated_absorpt_T_min    ?
_exptl_absorpt_coefficient_mu     0.892
_exptl_absorpt_correction_T_max   1.00000
_exptl_absorpt_correction_T_min   0.75479
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details    ?
_exptl_crystal_colour             'clear light yellow'
_exptl_crystal_colour_lustre      clear
_exptl_crystal_colour_modifier    light
_exptl_crystal_colour_primary     yellow
_exptl_crystal_density_diffrn     1.385
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_description        block
_exptl_crystal_F_000              426
_exptl_crystal_size_max           0.118
_exptl_crystal_size_mid           0.094
_exptl_crystal_size_min           0.09
_exptl_transmission_factor_max    ?
_exptl_transmission_factor_min    ?
_diffrn_reflns_av_R_equivalents   0.0630
_diffrn_reflns_av_unetI/netI      0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_number             8831
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full         25.000
_diffrn_reflns_theta_max          25.000
_diffrn_reflns_theta_min          1.925
_diffrn_ambient_temperature       150
_diffrn_detector                  CCD
_diffrn_detector_area_resol_mean  28.5714
_diffrn_detector_type             'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω   -110.00  70.00   0.50    8.00    --  -20.00   0.00-180.00  360
  2  ω    -99.00  19.00   0.50    8.00    --  -20.00 -72.00-108.00  236
  3  ω   -106.50  19.00   0.50    8.00    --  -20.00 -72.00  36.00  251
  4  ω    -41.50 -33.50   0.50    8.00    --  -20.00  72.00-180.00   16
;
_diffrn_measurement_device        'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type   'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method        'profile data from ω-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11       -0.0496934000
_diffrn_orient_matrix_UB_12       0.0305551000
_diffrn_orient_matrix_UB_13       0.0237634000
_diffrn_orient_matrix_UB_21       -0.0503803000
_diffrn_orient_matrix_UB_22       -0.0222889000
_diffrn_orient_matrix_UB_23       -0.0623395000
_diffrn_orient_matrix_UB_31       -0.0378530000
_diffrn_orient_matrix_UB_32       -0.0623756000
_diffrn_orient_matrix_UB_33       0.0066829000
_diffrn_radiation_collimation     0.3
_diffrn_radiation_monochromator   Confocal
_diffrn_radiation_probe           x-ray
_diffrn_radiation_type            MoK\a
_diffrn_radiation_wavelength      0.71073
_diffrn_source                    'Rotating Anode'
_diffrn_source_current            24.0
_diffrn_source_power              1.2
_diffrn_source_target             Mo
_diffrn_source_type               'Rotating Anode'
_diffrn_source_voltage            50.0
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_full     .
_reflns_Friedel_fraction_max      .
_reflns_number_gt                 3443
_reflns_number_total              3701
_reflns_odcompleteness_completeness 87.98
_reflns_odcompleteness_iscentric  1
_reflns_odcompleteness_theta      31.03
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression      'I > 2σ(I)'
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement   'ShelXL (Sheldrick, 2008)'
_computing_structure_solution     ?
_refine_diff_density_max          1.136
_refine_diff_density_min          -1.134
_refine_diff_density_rms          0.257
_refine_ls_extinction_coef        .
_refine_ls_extinction_method      none
_refine_ls_goodness_of_fit_ref    1.224
_refine_ls_hydrogen_treatment     undef
_refine_ls_matrix_type            full
_refine_ls_number_parameters      253
_refine_ls_number_reflns          3701
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0505
_refine_ls_R_factor_gt            0.0426
_refine_ls_restrained_S_all       1.224
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0735P)²+2.4003P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.1244
_refine_ls_wR_factor_ref          0.1391
_refine_special_details           ?
_olex2_refinement_description
;
;
_atom_sites_solution_hydrogens    .
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Pd00 Pd 0.39100(4) 0.66247(3) 0.44691(3) 0.01723(16) Uani 1 1 d . . . . .
 C002 C 0.2429(5) 0.3645(5) 0.3988(5) 0.0224(10) Uani 1 1 d . . . . .
 O003 O 0.4046(5) 0.6665(5) 0.0925(4) 0.0512(13) Uani 1 1 d . . . . .
 C004 C 0.2630(5) 0.4672(5) 0.3444(4) 0.0180(10) Uani 1 1 d . . . . .
 C006 C 0.2127(6) 0.5392(5) 0.1529(5) 0.0245(11) Uani 1 1 d . . . . .
 C008 C 0.1630(6) 0.2285(5) 0.3244(5) 0.0280(12) Uani 1 1 d . . . . .
 N009 N 0.5495(5) 0.8623(4) 0.5389(4) 0.0218(9) Uani 1 1 d . . . . .
 C00A C 0.4280(6) 0.6390(7) 0.7014(5) 0.0341(13) Uani 1 1 d . . . . .
 C00B C 0.2001(5) 0.4285(5) 0.2127(4) 0.0193(10) Uani 1 1 d . . . . .
 C00C C 0.8533(7) 1.0446(6) 0.4358(6) 0.0375(14) Uani 1 1 d . . . . .
 N00D N 0.4610(5) 0.6914(4) 0.3019(4) 0.0205(9) Uani 1 1 d . . . . .
 C00E C 0.3725(6) 0.6357(5) 0.1795(5) 0.0250(11) Uani 1 1 d . . . . .
 C00F C 0.3889(7) 0.6224(9) 0.8048(6) 0.0462(17) Uani 1 1 d . . . . .
 C00G C 0.5837(6) 0.9481(5) 0.6561(5) 0.0279(12) Uani 1 1 d . . . . .
 C00H C 0.1422(7) 0.6178(8) 0.7041(6) 0.0451(17) Uani 1 1 d . . . . .
 N00I N 0.3285(5) 0.6432(5) 0.6006(4) 0.0219(9) Uani 1 1 d . . . . .
 C00J C 0.7983(6) 1.1052(5) 0.6412(6) 0.0331(13) Uani 1 1 d . . . . .
 C00K C 0.7653(6) 1.0168(5) 0.5137(5) 0.0287(12) Uani 1 1 d . . . . .
 C00L C 0.6854(6) 0.8314(6) 0.2668(5) 0.0345(13) Uani 1 1 d . . . . .
 C00M C 0.1011(6) 0.1918(5) 0.1937(5) 0.0303(12) Uani 1 1 d . . . . .
 C00N C 0.7072(7) 1.0702(6) 0.7102(5) 0.0354(14) Uani 1 1 d . . . . .
 C00O C 0.8135(7) 0.9529(7) 0.3150(6) 0.0395(14) Uani 1 1 d . . . . .
 C00P C 0.1202(6) 0.2915(5) 0.1372(5) 0.0243(11) Uani 1 1 d . . . . .
 C00Q C 0.2440(7) 0.6114(9) 0.8074(6) 0.0517(19) Uani 1 1 d . . . . .
 C00R C 0.1875(6) 0.6331(6) 0.6033(5) 0.0300(12) Uani 1 1 d . . . . .
 C00S C 0.0490(8) 0.2463(6) -0.0063(5) 0.0429(16) Uani 1 1 d . . . . .
 C00U C 0.6375(6) 0.8953(5) 0.4672(5) 0.0228(10) Uani 1 1 d . . . . .
 C00V C 0.5947(6) 0.8019(5) 0.3401(5) 0.0246(11) Uani 1 1 d . . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Pd00 C004 1.999(5) . ?
 Pd00 N009 2.104(4) . ?
 Pd00 N00D 2.015(4) . ?
 Pd00 N00I 2.048(4) . ?
 C002 C004 1.403(7) . ?
 C002 C008 1.382(8) . ?
 O003 C00E 1.220(6) . ?
 C004 C00B 1.406(7) . ?
 C006 C00B 1.521(7) . ?
 C006 C00E 1.530(7) . ?
 C008 C00M 1.397(8) . ?
 N009 C00G 1.329(7) . ?
 N009 C00U 1.365(7) . ?
 C00A C00F 1.377(8) . ?
 C00A N00I 1.351(7) . ?
 C00B C00P 1.393(7) . ?
 C00C C00K 1.410(9) . ?
 C00C C00O 1.377(9) . ?
 N00D C00E 1.353(6) . ?
 N00D C00V 1.394(7) . ?
 C00F C00Q 1.379(9) . ?
 C00G C00N 1.396(8) . ?
 C00H C00Q 1.395(9) . ?
 C00H C00R 1.371(8) . ?
 N00I C00R 1.343(7) . ?
 C00J C00K 1.435(8) . ?
 C00J C00N 1.365(9) . ?
 C00K C00U 1.417(7) . ?
 C00L C00O 1.418(8) . ?
 C00L C00V 1.388(8) . ?
 C00M C00P 1.392(7) . ?
 C00P C00S 1.532(7) . ?
 C00U C00V 1.436(7) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 C004 Pd00 N009 170.96(17) . . ?
 C004 Pd00 N00D 92.40(18) . . ?
 C004 Pd00 N00I 90.68(18) . . ?
 N00D Pd00 N009 80.26(16) . . ?
 N00D Pd00 N00I 176.88(15) . . ?
 N00I Pd00 N009 96.63(17) . . ?
 C008 C002 C004 120.6(5) . . ?
 C002 C004 Pd00 121.8(4) . . ?
 C002 C004 C00B 118.4(5) . . ?
 C00B C004 Pd00 119.7(3) . . ?
 C00B C006 C00E 116.4(4) . . ?
 C002 C008 C00M 120.3(5) . . ?
 C00G N009 Pd00 129.7(4) . . ?
 C00G N009 C00U 118.8(5) . . ?
 C00U N009 Pd00 111.0(3) . . ?
 N00I C00A C00F 122.3(5) . . ?
 C004 C00B C006 119.2(4) . . ?
 C00P C00B C004 121.2(4) . . ?
 C00P C00B C006 119.5(4) . . ?
 C00O C00C C00K 119.3(5) . . ?
 C00E N00D Pd00 124.2(3) . . ?
 C00E N00D C00V 120.5(4) . . ?
 C00V N00D Pd00 113.3(3) . . ?
 O003 C00E C006 118.2(4) . . ?
 O003 C00E N00D 125.3(5) . . ?
 N00D C00E C006 116.1(4) . . ?
 C00A C00F C00Q 119.4(5) . . ?
 N009 C00G C00N 123.1(5) . . ?
 C00R C00H C00Q 119.7(5) . . ?
 C00A N00I Pd00 120.7(3) . . ?
 C00R N00I Pd00 121.0(3) . . ?
 C00R N00I C00A 118.3(4) . . ?
 C00N C00J C00K 119.7(5) . . ?
 C00C C00K C00J 123.5(5) . . ?
 C00C C00K C00U 119.8(5) . . ?
 C00U C00K C00J 116.7(5) . . ?
 C00V C00L C00O 120.8(5) . . ?
 C00P C00M C008 120.3(5) . . ?
 C00J C00N C00G 119.5(5) . . ?
 C00C C00O C00L 121.5(5) . . ?
 C00B C00P C00S 122.4(5) . . ?
 C00M C00P C00B 119.2(5) . . ?
 C00M C00P C00S 118.3(5) . . ?
 C00F C00Q C00H 118.2(5) . . ?
 N00I C00R C00H 122.1(5) . . ?
 N009 C00U C00K 122.4(5) . . ?
 N009 C00U C00V 117.1(4) . . ?
 C00K C00U C00V 120.5(5) . . ?
 N00D C00V C00U 115.3(5) . . ?
 C00L C00V N00D 126.6(5) . . ?
 C00L C00V C00U 118.0(5) . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 Pd00 C004 C00B C006 -8.3(6) . . . . ?
 Pd00 C004 C00B C00P 175.0(4) . . . . ?
 Pd00 N009 C00G C00N 170.3(4) . . . . ?
 Pd00 N009 C00U C00K -171.8(4) . . . . ?
 Pd00 N009 C00U C00V 8.8(5) . . . . ?
 Pd00 N00D C00E O003 169.1(5) . . . . ?
 Pd00 N00D C00E C006 -3.4(6) . . . . ?
 Pd00 N00D C00V C00L 166.8(5) . . . . ?
 Pd00 N00D C00V C00U -15.4(5) . . . . ?
 Pd00 N00I C00R C00H 178.9(5) . . . . ?
 C002 C004 C00B C006 176.5(4) . . . . ?
 C002 C004 C00B C00P -0.3(7) . . . . ?
 C002 C008 C00M C00P 0.5(8) . . . . ?
 C004 C002 C008 C00M -0.1(8) . . . . ?
 C004 C00B C00P C00M 0.7(8) . . . . ?
 C004 C00B C00P C00S 179.3(5) . . . . ?
 C006 C00B C00P C00M -176.0(5) . . . . ?
 C006 C00B C00P C00S 2.6(8) . . . . ?
 C008 C002 C004 Pd00 -175.2(4) . . . . ?
 C008 C002 C004 C00B 0.0(7) . . . . ?
 C008 C00M C00P C00B -0.8(8) . . . . ?
 C008 C00M C00P C00S -179.5(6) . . . . ?
 N009 C00G C00N C00J 0.2(8) . . . . ?
 N009 C00U C00V N00D 4.0(6) . . . . ?
 N009 C00U C00V C00L -178.0(5) . . . . ?
 C00A C00F C00Q C00H 0.0(13) . . . . ?
 C00A N00I C00R C00H -0.5(9) . . . . ?
 C00B C006 C00E O003 138.4(6) . . . . ?
 C00B C006 C00E N00D -48.6(7) . . . . ?
 C00C C00K C00U N009 179.1(5) . . . . ?
 C00C C00K C00U C00V -1.5(7) . . . . ?
 C00E C006 C00B C004 55.9(6) . . . . ?
 C00E C006 C00B C00P -127.3(5) . . . . ?
 C00E N00D C00V C00L -28.6(8) . . . . ?
 C00E N00D C00V C00U 149.2(5) . . . . ?
 C00F C00A N00I Pd00 -178.2(6) . . . . ?
 C00F C00A N00I C00R 1.2(9) . . . . ?
 C00G N009 C00U C00K 0.9(7) . . . . ?
 C00G N009 C00U C00V -178.5(4) . . . . ?
 N00I C00A C00F C00Q -1.0(12) . . . . ?
 C00J C00K C00U N009 -0.3(7) . . . . ?
 C00J C00K C00U C00V 179.1(5) . . . . ?
 C00K C00C C00O C00L 0.3(9) . . . . ?
 C00K C00J C00N C00G 0.5(8) . . . . ?
 C00K C00U C00V N00D -175.5(4) . . . . ?
 C00K C00U C00V C00L 2.5(7) . . . . ?
 C00N C00J C00K C00C -179.8(5) . . . . ?
 C00N C00J C00K C00U -0.4(7) . . . . ?
 C00O C00C C00K C00J 179.4(5) . . . . ?
 C00O C00C C00K C00U 0.0(8) . . . . ?
 C00O C00L C00V N00D 175.6(5) . . . . ?
 C00O C00L C00V C00U -2.2(8) . . . . ?
 C00Q C00H C00R N00I -0.5(11) . . . . ?
 C00R C00H C00Q C00F 0.7(12) . . . . ?
 C00U N009 C00G C00N -0.9(7) . . . . ?
 C00V N00D C00E O003 6.3(9) . . . . ?
 C00V N00D C00E C006 -166.2(5) . . . . ?
 C00V C00L C00O C00C 0.8(9) . . . . ?

_shelx_SHELXL_version_number      '2014/7'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.433
_oxdiff_exptl_absorpt_empirical_full_min 0.837
