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_7033678
_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
'C112 H92 Cl2 Fe2 N20 Zn2, 6(F6 P), C4 H8 O2, 2(O)'
_chemical_formula_sum            'C116 H100 Cl2 F36 Fe2 N20 O4 P6 Zn2'
_chemical_formula_weight         3021.31
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_audit_update_record
;
2015-01-16 deposited with the CCDC.
2015-01-16 downloaded from the CCDC.
;
_cell_angle_alpha                76.066(4)
_cell_angle_beta                 83.142(4)
_cell_angle_gamma                82.373(4)
_cell_formula_units_Z            1
_cell_length_a                   12.8625(5)
_cell_length_b                   14.2812(7)
_cell_length_c                   18.9563(9)
_cell_measurement_reflns_used    8973
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      73.8154
_cell_measurement_theta_min      3.2007
_cell_volume                     3335.9(3)
_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_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6501
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
  1 omega -120.00    6.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.7813  -19.0000   60.0000 126

  2 omega -114.00  -78.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.7813 -135.0000   83.0000 36

  3 omega  -38.00   36.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.7813   37.0000   60.0000 74

  4 omega    7.00   80.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       39.7813  -99.0000  -30.0000 73

  5 omega   23.00   49.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       39.7813 -125.0000  -30.0000 26

  6 omega   45.00   74.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       39.7813 -134.0000  -96.0000 29

  7 omega   42.00   96.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       39.7813 -125.0000  150.0000 54

  8 omega -128.00 -100.00   1.0000   27.2500
omega____ theta____ kappa____ phi______ frames
    -      -61.5000 -125.0000 -180.0000 28

  9 omega   32.00  108.00   1.0000   27.2500
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -94.0000 -120.0000 76

 10 omega   48.00  109.00   1.0000   27.2500
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -94.0000  150.0000 61

 11 omega   40.00   84.00   1.0000   27.2500
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000  -30.0000 44

 12 omega   34.00   65.00   1.0000   27.2500
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000  -30.0000 31

 13 omega   35.00   89.00   1.0000   27.2500
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -30.0000   60.0000 54

 14 omega   54.00  161.00   1.0000   27.2500
omega____ theta____ kappa____ phi______ frames
    -      107.7801   15.0000  -90.0000 107

 15 omega   66.00   93.00   1.0000   27.2500
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -94.0000   90.0000 27

 16 omega   62.00  117.00   1.0000   27.2500
omega____ theta____ kappa____ phi______ frames
    -      107.7801 -125.0000   90.0000 55

 17 omega  141.00  169.00   1.0000   27.2500
omega____ theta____ kappa____ phi______ frames
    -      107.7801   30.0000  -30.0000 28

 18 omega   78.00  116.00   1.0000   27.2500
omega____ theta____ kappa____ phi______ frames
    -      107.7801   30.0000  -30.0000 38

 19 omega   34.00   84.00   1.0000   27.2500
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000   30.0000 50

 20 omega   33.00   91.00   1.0000   27.2500
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -94.0000  -30.0000 58

 21 omega   38.00   91.00   1.0000   27.2500
omega____ theta____ kappa____ phi______ frames
    -      107.7801  -45.0000  120.0000 53

 22 omega  124.00  178.00   1.0000   27.2500
omega____ theta____ kappa____ phi______ frames
    -      107.7801   61.0000  120.0000 54

 23 omega  112.00  165.00   1.0000   27.2500
omega____ theta____ kappa____ phi______ frames
    -      107.7801  125.0000   30.0000 53

 24 omega  -69.00   -6.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.7813  -77.0000  -60.0000 63

 25 omega -118.00   -6.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.7813  -77.0000    0.0000 112

 26 omega -114.00  -10.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.7813  -57.0000   30.0000 104

 27 omega    1.00   82.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       39.7813  -99.0000  -60.0000 81

 28 omega    1.00   82.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       39.7813  -99.0000  150.0000 81

 29 omega    6.00  118.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       39.7813   77.0000 -150.0000 112

 30 omega   77.00  178.00   1.0000   27.2500
omega____ theta____ kappa____ phi______ frames
    -      107.7801   30.0000   60.0000 101
;
_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      0.0496300335
_diffrn_orient_matrix_UB_12      -0.0811931424
_diffrn_orient_matrix_UB_13      -0.0381839546
_diffrn_orient_matrix_UB_21      -0.0131230998
_diffrn_orient_matrix_UB_22      0.0700131069
_diffrn_orient_matrix_UB_23      -0.0749108178
_diffrn_orient_matrix_UB_31      0.1099489375
_diffrn_orient_matrix_UB_32      0.0316933505
_diffrn_orient_matrix_UB_33      -0.0001402755
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33723
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.982
_diffrn_reflns_theta_min         3.207
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.120
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.532
_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    1.504
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_recrystallization_method 'Vapour Deposition'
_exptl_crystal_size_max          0.1988
_exptl_crystal_size_mid          0.0519
_exptl_crystal_size_min          0.0309
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     933
_refine_ls_number_reflns         13087
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0820P)^2^+1.9715P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9566
_reflns_number_total             13087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03089c2.cif
_cod_data_source_block           gka26a
_cod_depositor_comments
'Adding full bibliography for 7033678--7033682.cif.'
_cod_database_code               7033678
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         C58H51N10Cl1P3F18Fe1Zn1
_reflns_odcompleteness_completeness 99.79
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N27-H27
 0.9 with sigma of 0.02
 N43-H43
 0.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C74) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C69) = Uanis(C75)
4. Others
 Fixed Sof: O79(0.3) O77(0.3) O71(0.2) C80(0.3) H80A(0.3) H80B(0.3) H80C(0.3)
 C78(0.3) C76(0.3) H76A(0.3) H76B(0.3) O73(0.2) C69(0.2) H69A(0.2) H69B(0.2)
 H69C(0.2) C72(0.2) C70(0.2) H70A(0.2) H70B(0.2) C74(0.2) H74A(0.2) H74B(0.2)
 H74C(0.2) C75(0.3) H75A(0.3) H75B(0.3) H75C(0.3) O102(0.5) O103(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C42(H42A,H42B), C44(H44A,H44B), C28(H28A,H28B), C76(H76A,
 H76B), C70(H70A,H70B)
5.b Aromatic/amide H refined with riding coordinates:
 C58(H58), C60(H60), C9(H9), C52(H52), C15(H15), C11(H11), C24(H24), C55(H55),
 C18(H18), C46(H46), C6(H6), C3(H3), C54(H54), C4(H4), C17(H17), C67(H67),
 C21(H21), C16(H16), C22(H22), C64(H64), C47(H47), C40(H40), C5(H5), C65(H65),
 C49(H49), C53(H53), C23(H23), C48(H48), C37(H37), C33(H33), C66(H66), C39(H39),
  C38(H38), C31(H31), C32(H32), C30(H30)
5.c Idealised Me refined as rotating group:
 C80(H80A,H80B,H80C), C69(H69A,H69B,H69C), C74(H74A,H74B,H74C), C75(H75A,H75B,
 H75C)
;
_olex2_submission_special_instructions 'No special instructions were received'