Deliberate boxes and accidental wheels.
Kaur, Gurpreet; Polson, Matthew I. J.; Hartshorn, Richard M.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 4200–4206; doi:10.1039/c4dt03089c

data_7033682
_publ_section_title
;
 Deliberate boxes and accidental wheels.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4200
_journal_page_last               4206
_journal_paper_doi               10.1039/c4dt03089c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C58 H49 N10 O2 Zn2, 3(F6 P), C2 H3 N'
_chemical_formula_sum            'C60 H52 F18 N11 O2 P3 Zn2'
_chemical_formula_weight         1524.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-03-27
_audit_creation_method
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Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4813)
;
_audit_update_record
;
2014-12-14 deposited with the CCDC.
2015-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.638(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.189(2)
_cell_length_b                   14.8680(6)
_cell_length_c                   26.4641(16)
_cell_measurement_reflns_used    3437
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.6281
_cell_measurement_theta_min      2.6642
_cell_volume                     13040.4(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -48.00   20.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6615   37.0000  -60.0000 68

  2 omega  -47.00  -10.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6615   37.0000  -90.0000 37

  3 omega -116.00  -24.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.6615  -37.0000  -60.0000 92

  4 omega   57.00   97.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       39.6615 -139.0000 -142.0000 40

  5 omega   46.00   93.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7749   15.0000 -180.0000 47

  6 omega   94.00  159.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7749   30.0000   60.0000 65

  7 omega   30.00   82.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7749  -30.0000  -90.0000 52

  8 omega   90.00  110.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7749 -125.0000 -180.0000 20

  9 omega   54.00  109.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7749  -94.0000 -150.0000 55

 10 omega   35.00   92.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7749  -45.0000  150.0000 57

 11 omega   33.00   94.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7749  -45.0000 -150.0000 61

 12 omega  101.00  168.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7749   15.0000 -180.0000 67

 13 omega  130.00  176.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      107.7749  125.0000  -90.0000 46
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0173562000
_diffrn_orient_matrix_UB_12      -0.0032305000
_diffrn_orient_matrix_UB_13      0.0617513000
_diffrn_orient_matrix_UB_21      0.0430774000
_diffrn_orient_matrix_UB_22      -0.0024005000
_diffrn_orient_matrix_UB_23      -0.0025713000
_diffrn_orient_matrix_UB_31      0.0014376000
_diffrn_orient_matrix_UB_32      0.1035119000
_diffrn_orient_matrix_UB_33      0.0018093000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0882
_diffrn_reflns_av_unetI/netI     0.1372
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25940
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.496
_diffrn_reflns_theta_min         2.666
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.523
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       irregular
_exptl_crystal_F_000             6176
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     867
_refine_ls_number_reflns         11241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1272
_refine_ls_R_factor_gt           0.0702
_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/[\s^2^(Fo^2^)+(0.0705P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.2280
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6177
_reflns_number_total             11241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03089c2.cif
_cod_data_source_block           gka21
_cod_depositor_comments
'Adding full bibliography for 7033678--7033682.cif.'
_cod_original_cell_volume        13040.6(14)
_cod_database_code               7033682
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         C20H20N4O4F6P1ZN1
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N9(H9), N7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C51(H51A,H51B), C22(H22A,H22B), C23(H23A,H23B)
2.c Aromatic/amide H refined with riding coordinates:
 C35(H35), C12(H12), C40(H40), C54(H54), C9(H9A), C45(H45), C2(H2), C1(H1),
 C53(H53), C43(H43), C47(H47), C32(H32), C7(H7A), C37(H37), C56(H56), C48(H48),
 C41(H41), C27(H27), C26(H26), C19(H19), C28(H28), C17(H17), C55(H55), C4(H4),
 C46(H46), C29(H29), C30(H30), C18(H18), C15(H15), C25(H25), C14(H14), C31(H31),
  C13(H13), C42(H42), C3(H3), C20(H20)
2.d Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C), C60(H60A,H60B,H60C)
;
_shelx_res_checksum              33680
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'