data_mo_68301_0m_a_sq
_audit_creation_date               2019-06-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2017/1'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_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          PFC-17
_chemical_formula_moiety           '0.13(C160 H96 N72 O32 Zn16)'
_chemical_formula_sum              'C11.75 H11.75 N11.75 O11.75 Zn11.75'
_chemical_formula_weight           1273.68
_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'
 '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'
 'Zn' 'Zn' 0.2839 1.4301 '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        'tetragonal'
_space_group_IT_number             87
_space_group_name_H-M_alt          'I 4/m'
_space_group_name_Hall             '-I 4'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z'
 '-y, x, z'
 'y, -x, z'
 'x+1/2, y+1/2, z+1/2'
 '-x+1/2, -y+1/2, z+1/2'
 '-y+1/2, x+1/2, z+1/2'
 'y+1/2, -x+1/2, z+1/2'
 '-x, -y, -z'
 'x, y, -z'
 'y, -x, -z'
 '-y, x, -z'
 '-x+1/2, -y+1/2, -z+1/2'
 'x+1/2, y+1/2, -z+1/2'
 'y+1/2, -x+1/2, -z+1/2'
 '-y+1/2, x+1/2, -z+1/2'

_cell_length_a                     13.3591(19)
_cell_length_b                     13.3591(19)
_cell_length_c                     42.446(5)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       7575(2)
_cell_formula_units_Z              8
_cell_measurement_reflns_used      9991
_cell_measurement_temperature      100(2)
_cell_measurement_theta_max        25.37
_cell_measurement_theta_min        2.36
_shelx_estimated_absorpt_T_max     0.527
_shelx_estimated_absorpt_T_min     0.307
_exptl_absorpt_coefficient_mu      7.351
_exptl_absorpt_correction_T_max    0.7456
_exptl_absorpt_correction_T_min    0.5984
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details    
 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0817 before and 0.0430 after correction. The Ratio of minimum to maximum transmission is 0.8026. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              colourless
_exptl_crystal_colour_primary      colourless
_exptl_crystal_density_diffrn      2.234
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         plate
_exptl_crystal_F_000               4888
_exptl_crystal_size_max            0.21
_exptl_crystal_size_mid            0.21
_exptl_crystal_size_min            0.1
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0680
_diffrn_reflns_av_unetI/netI       0.0305
_diffrn_reflns_Laue_measured_fraction_full  0.996
_diffrn_reflns_Laue_measured_fraction_max  0.996
_diffrn_reflns_limit_h_max         15
_diffrn_reflns_limit_h_min         -16
_diffrn_reflns_limit_k_max         15
_diffrn_reflns_limit_k_min         -16
_diffrn_reflns_limit_l_max         50
_diffrn_reflns_limit_l_min         -50
_diffrn_reflns_number              24110
_diffrn_reflns_point_group_measured_fraction_full  0.996
_diffrn_reflns_point_group_measured_fraction_max  0.996
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           25.321
_diffrn_reflns_theta_min           2.156
_diffrn_ambient_temperature        100.01
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.996
_diffrn_measured_fraction_theta_max  0.996
_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           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  3133
_reflns_number_total               3509
_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         'SAINT V8.38A (?, 2016)'
_computing_data_collection         ?
_computing_data_reduction          'SAINT V8.38A (?, 2016)'
_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      'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max           2.761
_refine_diff_density_min           -1.820
_refine_diff_density_rms           0.132
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.080
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       108
_refine_ls_number_reflns           3509
_refine_ls_number_restraints       2
_refine_ls_R_factor_all            0.0898
_refine_ls_R_factor_gt             0.0846
_refine_ls_restrained_S_all        1.080
_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)+(0.0717P)²+125.5598P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.2140
_refine_ls_wR_factor_ref           0.2170
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained planarity
 N2, C1, N1, N1_$1, C1_$1
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
Uanis(N2) = Uanis(N3)
Uanis(N2) = Uanis(N1)
Uanis(C5) = Uanis(C6) = Uanis(C7) = Uanis(C2) = Uanis(C4) = Uanis(C3)
4.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C6(H6), C7(H7), C3(H3), C4(H4)
4.b Fitted hexagon refined as free rotating group:
 C5(C6,C7,C2,C3,C4)
;
_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
 Zn1 Zn 0.33746(5) 0.22571(5) 0.28444(2) 0.0282(3) Uani 1 1 d . . . . .
 N5 N 0.6417(4) 0.2754(3) 0.27276(11) 0.0284(10) Uani 1 1 d . . . . .
 N4 N 0.6254(4) 0.2112(4) 0.24794(10) 0.0279(10) Uani 1 1 d . . . . .
 N3 N 0.4822(7) 0.2325(7) 0.27279(15) 0.0784(15) Uani 1 1 d . . . . .
 O1 O 0.2932(5) 0.1712(4) 0.32428(11) 0.0582(14) Uani 1 1 d . . . . .
 O2 O 0.3853(4) 0.3024(5) 0.33733(11) 0.0599(15) Uani 1 1 d . . . . .
 C10 C 0.5552(4) 0.2873(4) 0.28683(13) 0.0292(12) Uani 1 1 d . . . . .
 H10 H 0.544834 0.329195 0.304631 0.035 Uiso 1 1 calc R . . . .
 C9 C 0.5301(4) 0.1885(4) 0.24911(14) 0.0319(13) Uani 1 1 d . . . . .
 H9 H 0.498408 0.144894 0.234505 0.038 Uiso 1 1 calc R . . . .
 C8 C 0.3305(7) 0.2316(8) 0.34485(18) 0.065(2) Uani 1 1 d . . . . .
 C5 C 0.3057(9) 0.2136(9) 0.37870(10) 0.151(3) Uani 1 1 d . . . . .
 C6 C 0.3510(8) 0.2713(8) 0.40195(14) 0.151(3) Uani 1 1 d G . . . .
 H6 H 0.399465 0.320145 0.396350 0.182 Uiso 1 1 calc R . . . .
 C7 C 0.3253(9) 0.2574(8) 0.43338(12) 0.151(3) Uani 1 1 d G . . . .
 H7 H 0.356203 0.296811 0.449264 0.182 Uiso 1 1 calc R . . . .
 C2 C 0.2543(9) 0.1859(9) 0.44157(10) 0.151(3) Uani 1 1 d G . . . .
 C3 C 0.2090(8) 0.1283(8) 0.41832(14) 0.151(3) Uani 1 1 d G . . . .
 H3 H 0.160544 0.079377 0.423920 0.182 Uiso 1 1 calc R . . . .
 C4 C 0.2347(8) 0.1421(8) 0.38689(12) 0.151(3) Uani 1 1 d G . . . .
 H4 H 0.203804 0.102711 0.371006 0.182 Uiso 1 1 calc R . . . .
 N1 N 0.1586(7) 0.1097(7) 0.48375(15) 0.0784(15) Uani 1 1 d . . . . .
 N2 N 0.2941(10) 0.1900(9) 0.500000 0.0784(15) Uani 1 2 d S T P . .
 C1 C 0.2346(12) 0.1583(11) 0.4751(2) 0.172(10) 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
 Zn1 N5 2.018(5) 4_565 ?
 Zn1 N4 2.026(5) 16_545 ?
 Zn1 N3 1.998(9) . ?
 Zn1 O1 1.934(5) . ?
 Zn1 C8 2.567(8) . ?
 N5 N4 1.375(6) . ?
 N5 C10 1.311(7) . ?
 N4 C9 1.311(7) . ?
 N3 C10 1.357(10) . ?
 N3 C9 1.328(10) . ?
 O1 C8 1.289(11) . ?
 O2 C8 1.238(11) . ?
 C10 H10 0.9500 . ?
 C9 H9 0.9500 . ?
 C8 C5 1.494(9) . ?
 C5 C6 1.3900 . ?
 C5 C4 1.3900 . ?
 C6 H6 0.9500 . ?
 C6 C7 1.3900 . ?
 C7 H7 0.9500 . ?
 C7 C2 1.3900 . ?
 C2 C3 1.3900 . ?
 C2 C1 1.495(12) . ?
 C3 H3 0.9500 . ?
 C3 C4 1.3900 . ?
 C4 H4 0.9500 . ?
 N1 N1 1.379(13) 10_556 ?
 N1 C1 1.259(16) . ?
 N2 C1 1.388(14) 10_556 ?
 N2 C1 1.388(14) . ?

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
 N5 Zn1 N4 106.36(19) 4_565 16_545 ?
 N5 Zn1 C8 101.8(3) 4_565 . ?
 N4 Zn1 C8 133.3(3) 16_545 . ?
 N3 Zn1 N5 107.3(3) . 4_565 ?
 N3 Zn1 N4 100.0(3) . 16_545 ?
 N3 Zn1 C8 106.3(3) . . ?
 O1 Zn1 N5 114.8(2) . 4_565 ?
 O1 Zn1 N4 104.2(2) . 16_545 ?
 O1 Zn1 N3 122.0(3) . . ?
 O1 Zn1 C8 29.2(3) . . ?
 N4 N5 Zn1 125.7(4) . 3_655 ?
 C10 N5 Zn1 127.7(4) . 3_655 ?
 C10 N5 N4 106.6(4) . . ?
 N5 N4 Zn1 128.0(4) . 15 ?
 C9 N4 Zn1 126.4(4) . 15 ?
 C9 N4 N5 105.6(4) . . ?
 C10 N3 Zn1 127.6(6) . . ?
 C9 N3 Zn1 129.3(6) . . ?
 C9 N3 C10 103.0(7) . . ?
 C8 O1 Zn1 103.8(5) . . ?
 N5 C10 N3 111.6(6) . . ?
 N5 C10 H10 124.2 . . ?
 N3 C10 H10 124.2 . . ?
 N4 C9 N3 113.2(6) . . ?
 N4 C9 H9 123.4 . . ?
 N3 C9 H9 123.4 . . ?
 O1 C8 Zn1 47.0(4) . . ?
 O1 C8 C5 117.7(8) . . ?
 O2 C8 Zn1 75.2(4) . . ?
 O2 C8 O1 122.2(7) . . ?
 O2 C8 C5 120.1(8) . . ?
 C5 C8 Zn1 164.5(7) . . ?
 C6 C5 C8 119.8(6) . . ?
 C6 C5 C4 120.0 . . ?
 C4 C5 C8 120.2(6) . . ?
 C5 C6 H6 120.0 . . ?
 C5 C6 C7 120.0 . . ?
 C7 C6 H6 120.0 . . ?
 C6 C7 H7 120.0 . . ?
 C2 C7 C6 120.0 . . ?
 C2 C7 H7 120.0 . . ?
 C7 C2 C3 120.0 . . ?
 C7 C2 C1 121.9(7) . . ?
 C3 C2 C1 117.6(7) . . ?
 C2 C3 H3 120.0 . . ?
 C4 C3 C2 120.0 . . ?
 C4 C3 H3 120.0 . . ?
 C5 C4 H4 120.0 . . ?
 C3 C4 C5 120.0 . . ?
 C3 C4 H4 120.0 . . ?
 C1 N1 N1 106.9(6) . 10_556 ?
 C1 N2 C1 99.0(14) . 10_556 ?
 N1 C1 C2 123.1(10) . . ?
 N1 C1 N2 113.5(10) . . ?
 N2 C1 C2 123.3(12) . . ?

_smtbx_masks_special_details       ?
loop_
  _smtbx_masks_void_nr
  _smtbx_masks_void_average_x
  _smtbx_masks_void_average_y
  _smtbx_masks_void_average_z
  _smtbx_masks_void_volume
  _smtbx_masks_void_count_electrons
  _smtbx_masks_void_content
 1 -0.432 -0.124 -0.579 4192.0 568.8 ?

_olex2_submission_special_instructions  'No special instructions were received'
