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_7033679
_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
'C120 H96 Fe2 N20 O4 Zn2, 5(F6 P), N O3, C2 H3 N'
_chemical_formula_sum            'C122 H99 F30 Fe2 N22 O7 P5 Zn2'
_chemical_formula_weight         2952.52
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-06-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.18 svn.r2945 for OlexSys, GUI svn.r4846)
;
_audit_update_record
;
2015-01-16 deposited with the CCDC.
2015-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.626(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9518(10)
_cell_length_b                   19.8601(6)
_cell_length_c                   36.0894(12)
_cell_measurement_reflns_used    9666
_cell_measurement_temperature    173.35(10)
_cell_measurement_theta_max      73.0410
_cell_measurement_theta_min      3.3450
_cell_volume                     14708.9(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.35(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3250
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
  1 omega -100.00  -22.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2539  -37.0000   30.0000 78

  2 omega   68.00   96.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2539 -125.0000  -90.0000 28

  3 omega  -79.00   -2.00   1.0000  230.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  125.0000  -30.0000 77

  4 omega  -54.00   15.00   1.0000  230.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000   45.0000 -120.0000 69

  5 omega   57.00   86.00   1.0000  230.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4325  -30.0000 -180.0000 29

  6 omega   98.00  157.00   1.0000  230.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4325  125.0000  -60.0000 59

  7 omega   56.00   86.00   1.0000  230.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4325  -30.0000  -30.0000 30

  8 omega   32.00   99.00   1.0000  230.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4325  -94.0000   30.0000 67

  9 omega   62.00  102.00   1.0000  230.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4325  -94.0000  120.0000 40

 10 omega   43.00   70.00   1.0000  230.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4325  -30.0000  -90.0000 27

 11 omega   84.00  178.00   1.0000  230.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4325   30.0000   30.0000 94

 12 omega   43.00   90.00   1.0000  230.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4325  -30.0000   60.0000 47

 13 omega   38.00   94.00   1.0000  230.0000
omega____ theta____ kappa____ phi______ frames
    -      107.4325  -45.0000   30.0000 56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0667684000
_diffrn_orient_matrix_UB_12      0.0150615000
_diffrn_orient_matrix_UB_13      -0.0099160000
_diffrn_orient_matrix_UB_21      -0.0100005000
_diffrn_orient_matrix_UB_22      0.0757108000
_diffrn_orient_matrix_UB_23      0.0060775000
_diffrn_orient_matrix_UB_31      0.0328557000
_diffrn_orient_matrix_UB_32      -0.0072724000
_diffrn_orient_matrix_UB_33      0.0420061000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            62630
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.428
_diffrn_reflns_theta_min         2.699
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.260
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.637
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       fragment
_exptl_crystal_F_000             5992
_exptl_crystal_recrystallization_method 'Vapour Deposition'
_exptl_crystal_size_max          0.1981
_exptl_crystal_size_mid          0.1494
_exptl_crystal_size_min          0.0135
_refine_diff_density_max         0.800
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1712
_refine_ls_number_reflns         28900
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1153P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1861
_refine_ls_wR_factor_ref         0.2075
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17013
_reflns_number_total             28900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03089c2.cif
_cod_data_source_block           gka116a
_cod_depositor_comments
'Adding full bibliography for 7033678--7033682.cif.'
_cod_database_code               7033679
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         C122H91N21O4F24P4FE2ZN2
_reflns_odcompleteness_completeness 99.67
_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. Restrained distances
 H32-N32
 0.9 with sigma of 0.02
 H20-N20
 0.9 with sigma of 0.02
 N91-H91
 0.9 with sigma of 0.02
 N48-H48
 0.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(N50) = Uiso(N50A)
4. Others
 Fixed Sof: F51(0.5) F52(0.5) F53(0.5) F54(0.5) F55(0.5) F56(0.5) P50(0.5)
 F61(0.5) F62(0.5) F64(0.5) F65(0.5) F66(0.5) P60(0.5) N50(0.5) O8(0.5)
 N50A(0.5) O169(0.5) F3(0.5)
 Fixed Uiso: F51(0.13) F52(0.13) F53(0.13) F54(0.13) F55(0.13) F56(0.13)
 P50(0.13) F61(0.11) F62(0.11) F64(0.11) F65(0.11) F66(0.11) P60(0.11) F3(0.11)
5.a Secondary CH2 refined with riding coordinates:
 C86(H86A,H86B), C103(H10A,H10B), C118(H11A,H11B), C119(H11C,H11D), C136(H13A,
 H13B), C137(H13C,H13D), C160(H16A,H16B), C167(H16C,H16D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C19(H19), C37(H37), C41(H41), C46(H46),
 C51(H51), C52(H52), C54(H54), C58(H58), C60(H60), C65(H65), C75(H75), C76(H76),
  C79(H79), C81(H81), C83(H83), C84(H84), C88(H88), C89(H89), C95(H95),
 C99(H99), C101(H101), C102(H102), C106(H106), C107(H107), C108(H108),
 C109(H109), C111(H111), C112(H112), C113(H113), C115(H115), C117(H117),
 C120(H120), C122(H122), C123(H123), C124(H124), C125(H125), C127(H127),
 C128(H128), C129(H129), C130(H130), C131(H131), C133(H133), C134(H134),
 C138(H138), C140(H140), C141(H141), C142(H142), C143(H143), C144(H144),
 C147(H147), C148(H148), C149(H149), C150(H150), C151(H151), C152(H152),
 C153(H153), C154(H154), C156(H156), C158(H158), C161(H161), C163(H163),
 C165(H165), C166(H166), C168(H168), C170(H170), C171(H171), C172(H172),
 C173(H173), C174(H174), C176(H176), C195(H195), C198(H198)
5.c Idealised Me refined as rotating group:
 C202(H20A,H20B,H20C)
;
_olex2_submission_special_instructions 'No special instructions were received'