Pentaarylcyclopentadienyl Iron, Cobalt, and Nickel Halides.
Chakraborty, Uttam; Modl, Moritz; Mühldorf, Bernd; Bodensteiner, Michael; Demeshko, Serhiy; van Velzen, Niels J. C.; Scheer, Manfred; Harder, Sjoerd; Wolf, Robert; Inorganic chemistry 55 (2016) 3065–3074; doi:10.1021/acs.inorgchem.5b02896

data_4347220
_publ_section_title
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 Pentaarylcyclopentadienyl Iron, Cobalt, and Nickel Halides.
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_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3065
_journal_page_last               3074
_journal_paper_doi               10.1021/acs.inorgchem.5b02896
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C98 H106 Br2 Fe2 O2, 3(C4 H8 O)'
_chemical_formula_sum            'C110 H130 Br2 Fe2 O5'
_chemical_formula_weight         1803.65
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_date             2014-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
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_cell_angle_alpha                76.5352(14)
_cell_angle_beta                 78.4800(14)
_cell_angle_gamma                65.6260(19)
_cell_formula_units_Z            2
_cell_length_a                   14.3360(3)
_cell_length_b                   14.4049(3)
_cell_length_c                   25.3801(4)
_cell_measurement_reflns_used    12590
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.2600
_cell_measurement_theta_min      12.1390
_cell_volume                     4610.97(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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      123.(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0921164000
_diffrn_orient_matrix_UB_12      0.0333350000
_diffrn_orient_matrix_UB_13      -0.0197853000
_diffrn_orient_matrix_UB_21      0.0277174000
_diffrn_orient_matrix_UB_22      -0.0286041000
_diffrn_orient_matrix_UB_23      0.0588384000
_diffrn_orient_matrix_UB_31      0.0697064000
_diffrn_orient_matrix_UB_32      -0.1107322000
_diffrn_orient_matrix_UB_33      -0.0097652000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            31477
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.569
_diffrn_reflns_theta_min         3.408
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.951
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.812
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1140
_refine_ls_number_reflns         31477
_refine_ls_number_restraints     314
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0893P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23323
_reflns_number_total             31477
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02896_si_002.cif
_cod_data_source_block           compound_1a
_cod_original_cell_volume        4610.95(16)
_cod_database_code               4347220
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         C45H45FeBr
_diffrn_oxdiff_twin_integration_method simultaneous
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C1C-C126
 1.51 with sigma of 0.01
 O7-C1C \\sim O7A-C1C \\sim O7A-C116 \\sim O7-C116 \\sim O9-C914 \\sim O9-C904
\\sim O9-C901 \\sim O2-C115
 \\sim O2-C122
 with sigma of 0.01
 C902-C901 \\sim C912-C901 \\sim C915-C912 \\sim C905-C902 \\sim C915-C914
\\sim C905-C904 \\sim C1C-
 C126 \\sim C126-C110 \\sim C116-C110 \\sim C122-C120 \\sim C1D-C120 \\sim
C1E-C120 \\sim C1E-C115 ~
 C1D-C115
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O7 \\sim C1C \\sim C116 \\sim O7A \\sim C126 \\sim C110 \\sim O9 \\sim C905
\\sim C902 \\sim C904 \\sim C901 \\sim C912 \\sim C914 \\sim C915 \\sim C120
\\sim O2 \\sim C115 \\sim C122 \\sim C1D \\sim C1E: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C1D(0.4) H1DA(0.4) H1DB(0.4) C1E(0.6) H1EA(0.6) H1EB(0.6)
 H11D(0.4) H11E(0.4) H11F(0.6) H11G(0.6) H12A(0.4) H12B(0.4) H12C(0.6)
 H12D(0.6) O7(0.6) O7A(0.4) H1CC(0.6) H1CD(0.6) H1CA(0.4) H1CB(0.4) H11L(0.6)
 H11M(0.6) H11J(0.4) H11K(0.4) C905(0.6) H90A(0.6) H90B(0.6) C915(0.4)
 H91D(0.4) H91E(0.4) H90E(0.6) H90F(0.6) H90C(0.4) H90D(0.4) C902(0.6)
 H90G(0.6) H90H(0.6) C904(0.6) H90I(0.6) H90J(0.6) C912(0.4) H91F(0.4)
 H91G(0.4) C914(0.4) H91H(0.4) H91I(0.4)
5.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C61(H61A,H61B), C64(H64A,H64B), C70(H70A,H70B), C71(H71A,
 H71B), C73(H73A,H73B), C75(H75A,H75B), C80(H80A,H80B), C82(H82A,H82B),
 C84(H84A,H84B), C88(H88A,H88B), C89(H89A,H89B), C95(H95A,H95B), C96(H96A,H96B),
  C102(H10F,H10G), C103(H10H,H10I), C1D(H1DA,H1DB), C1E(H1EA,H1EB), C115(H11D,
 H11E), C115(H11F,H11G), C120(H12A,H12B), C120(H12C,H12D), C122(H12E,H12F),
 C1C(H1CC,H1CD), C1C(H1CA,H1CB), C110(H11H,H11I), C116(H11L,H11M), C116(H11J,
 H11K), C126(H12G,H12H), C905(H90A,H90B), C915(H91D,H91E), C901(H90E,H90F),
 C901(H90C,H90D), C902(H90G,H90H), C904(H90I,H90J), C912(H91F,H91G), C914(H91H,
 H91I)
5.b Aromatic/amide H refined with riding coordinates:
 C1A(H1AA), C1B(H1BA), C10(H10), C14(H14), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C26(H26), C29(H29), C33(H33),
  C34(H34), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C47(H47),
 C49(H49), C50(H50), C52(H52), C53(H53), C59(H59), C60(H60), C62(H62), C66(H66),
  C68(H68), C72(H72), C76(H76), C81(H81), C85(H85), C86(H86), C90(H90),
 C92(H92), C99(H99), C900(H900)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C74(H74A,H74B,H74C), C77(H77A,H77B,H77C), C78(H78A,H78B,
 H78C), C87(H87A,H87B,H87C), C91(H91A,H91B,H91C), C93(H93A,H93B,H93C),
 C101(H10C,H10D,H10E), C107(H10J,H10K,H10L), C112(H11A,H11B,H11C)
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_shelx_res_checksum              85583
_shelx_hkl_checksum              92512