data_R,R_MCl2
_audit_creation_date              2020-02-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number      '2014/7'
_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. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common             ?
_chemical_name_systematic         ?
_chemical_formula_moiety          'C10 H22 Cl2 N2 Pd'
_chemical_formula_sum             'C10 H22 Cl2 N2 Pd'
_chemical_formula_weight          347.59
_chemical_absolute_configuration  ?
_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'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl' 'Cl' 0.1484 0.1585 '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'
 '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       'monoclinic'
_space_group_IT_number            5
_space_group_name_H-M_alt         'C 1 2 1'
_space_group_name_Hall            'C 2y'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z'

_cell_length_a                    8.5599(3)
_cell_length_b                    10.5975(4)
_cell_length_c                    7.9817(4)
_cell_angle_alpha                 90
_cell_angle_beta                  117.733(2)
_cell_angle_gamma                 90
_cell_volume                      640.87(5)
_cell_formula_units_Z             2
_cell_measurement_reflns_used     6360
_cell_measurement_temperature     298(2)
_cell_measurement_theta_max       31.58
_cell_measurement_theta_min       3.31
_shelx_estimated_absorpt_T_max    ?
_shelx_estimated_absorpt_T_min    ?
_exptl_absorpt_coefficient_mu     1.836
_exptl_absorpt_correction_T_max   0.7463
_exptl_absorpt_correction_T_min   0.5980
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0873 before and 0.0545 after correction.
The Ratio of minimum to maximum transmission is 0.8013.
The λ/2 correction factor is 0.0015.
;
_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     1.801
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_description        block
_exptl_crystal_F_000              352
_exptl_crystal_size_max           0.4
_exptl_crystal_size_mid           0.3
_exptl_crystal_size_min           0.3
_exptl_transmission_factor_max    ?
_exptl_transmission_factor_min    ?
_diffrn_reflns_av_R_equivalents   0.0359
_diffrn_reflns_av_unetI/netI      0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_l_max        9
_diffrn_reflns_limit_l_min        -9
_diffrn_reflns_number             7161
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full         24.994
_diffrn_reflns_theta_max          24.994
_diffrn_reflns_theta_min          3.305
_diffrn_ambient_temperature       298(2)
_diffrn_detector_area_resol_mean  ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type   'Bruker APEX-II CCD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_radiation_type            MoK\a
_diffrn_radiation_wavelength      0.71073
_diffrn_source                    ?
_diffrn_standards_number          0
_reflns_Friedel_coverage          0.889
_reflns_Friedel_fraction_full     1.000
_reflns_Friedel_fraction_max      1.000
_reflns_number_gt                 1123
_reflns_number_total              1128
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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        'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection        ?
_computing_data_reduction         'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement   'ShelXL (Sheldrick, 2015)'
_computing_structure_solution     ?
_refine_diff_density_max          0.355
_refine_diff_density_min          -0.306
_refine_diff_density_rms          0.061
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack    -0.01(6)
_refine_ls_extinction_coef        .
_refine_ls_extinction_method      none
_refine_ls_goodness_of_fit_ref    1.065
_refine_ls_hydrogen_treatment     constr
_refine_ls_matrix_type            full
_refine_ls_number_parameters      70
_refine_ls_number_reflns          1128
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0179
_refine_ls_R_factor_gt            0.0177
_refine_ls_restrained_S_all       1.064
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0196P)²+0.5940P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.0399
_refine_ls_wR_factor_ref          0.0399
_refine_special_details
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.01(6)
 -0.01(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C3(H3)
3.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B)
3.c Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens    geom
_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
 C9 C 0.0299(7) 0.0348(5) 0.3191(6) 0.0252(11) Uani 1 1 d . . . . .
 H9A H -0.0950 0.0470 0.2440 0.038 Uiso 1 1 calc R . . . .
 H9B H 0.0513 -0.0436 0.3867 0.038 Uiso 1 1 calc R . . . .
 H9C H 0.0785 0.1030 0.4076 0.038 Uiso 1 1 calc R . . . .
 C8 C 0.3065(7) 0.0125(5) 0.3191(7) 0.0286(12) Uani 1 1 d . . . . .
 H8A H 0.3664 0.0099 0.2430 0.043 Uiso 1 1 calc R . . . .
 H8B H 0.3522 0.0810 0.4076 0.043 Uiso 1 1 calc R . . . .
 H8C H 0.3250 -0.0656 0.3867 0.043 Uiso 1 1 calc R . . . .
 C11 C 0.0909(5) 0.3892(9) 0.0842(6) 0.0281(9) Uani 1 1 d . . . . .
 H11A H 0.1053 0.4641 0.1599 0.034 Uiso 1 1 calc R . . . .
 H11B H 0.1795 0.3912 0.0408 0.034 Uiso 1 1 calc R . . . .
 C12 C 0.1172(6) 0.2727(5) 0.2046(7) 0.0237(11) Uani 1 1 d . . . . .
 H12A H 0.0333 0.2733 0.2545 0.028 Uiso 1 1 calc R . . . .
 H12B H 0.2352 0.2733 0.3106 0.028 Uiso 1 1 calc R . . . .
 Pd1 Pd 0.0000 -0.11167(8) 0.0000 0.01310(14) Uani 1 2 d S T P . .
 Cl5 Cl 0.1229(4) -0.26650(10) 0.2287(3) 0.0253(5) Uani 1 1 d . . . . .
 N2 N 0.1139(10) 0.0316(5) 0.1947(8) 0.0145(14) Uani 1 1 d . . . . .
 C3 C 0.0914(6) 0.1530(4) 0.0863(6) 0.0173(10) Uani 1 1 d . . . . .
 H3 H 0.1795 0.1538 0.0404 0.021 Uiso 1 1 calc R . . . .


_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
 C9 N2 1.473(8) . ?
 C8 N2 1.490(8) . ?
 C11 C11 1.510(8) 2 ?
 C11 C12 1.515(9) . ?
 C12 C3 1.535(6) . ?
 Pd1 Cl5 2.3118(19) 2 ?
 Pd1 Cl5 2.3118(19) . ?
 Pd1 N2 2.064(6) . ?
 Pd1 N2 2.064(6) 2 ?
 N2 C3 1.512(7) . ?
 C3 C3 1.530(9) 2 ?

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
 C11 C11 C12 110.6(3) 2 . ?
 C11 C12 C3 110.3(4) . . ?
 Cl5 Pd1 Cl5 89.57(10) 2 . ?
 N2 Pd1 Cl5 92.60(13) . . ?
 N2 Pd1 Cl5 92.60(13) 2 2 ?
 N2 Pd1 Cl5 176.9(2) 2 . ?
 N2 Pd1 Cl5 176.9(2) . 2 ?
 N2 Pd1 N2 85.3(3) 2 . ?
 C9 N2 C8 106.9(5) . . ?
 C9 N2 Pd1 108.5(4) . . ?
 C9 N2 C3 113.2(5) . . ?
 C8 N2 Pd1 113.0(4) . . ?
 C8 N2 C3 107.7(5) . . ?
 C3 N2 Pd1 107.8(4) . . ?
 N2 C3 C12 114.1(4) . . ?
 N2 C3 C3 108.7(3) . 2 ?
 C3 C3 C12 110.4(3) 2 . ?


_olex2_submission_special_instructions 'No special instructions were received'
loop_
  _twin_individual_id
  _twin_individual_mass_fraction_refined
 1 1.01(6)
 2 -0.01(6)

