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_4347222
_publ_section_title
;
 Pentaarylcyclopentadienyl Iron, Cobalt, and Nickel Halides.
;
_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         'C90 H90 Br2 Co2, 0.5(C4 H8 O)'
_chemical_formula_sum            'C92 H94 Br2 Co2 O0.5'
_chemical_formula_weight         1485.35
_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   geom
_audit_creation_date             2015-10-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                99.1979(18)
_cell_angle_beta                 101.964(2)
_cell_angle_gamma                97.895(2)
_cell_formula_units_Z            2
_cell_length_a                   13.9761(4)
_cell_length_b                   15.3878(3)
_cell_length_c                   18.3949(4)
_cell_measurement_reflns_used    20126
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.5200
_cell_measurement_theta_min      4.2260
_cell_volume                     3760.33(16)
_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, 2015)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
  1 omega  -70.00   32.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5337   57.0000   60.0000 102

  2 omega  -70.00   35.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5337   77.0000  150.0000 105

  3 omega    8.00  108.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5337   77.0000  -90.0000 100

  4 omega   33.00  138.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -61.0000   90.0000 105

  5 omega   33.00   66.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -30.0000    0.0000 33

  6 omega   44.00  109.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -94.0000   90.0000 65

  7 omega   35.00   73.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -45.0000 -120.0000 38

  8 omega   61.00  152.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027   15.0000  -60.0000 91

  9 omega   69.00  108.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -94.0000 -180.0000 39

 10 omega   30.00   67.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -30.0000  -90.0000 37

 11 omega   32.00   69.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -30.0000  -60.0000 37

 12 omega   31.00   69.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -30.0000   30.0000 38

 13 omega   48.00  137.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -77.0000  -60.0000 89

 14 omega   48.00  154.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027   15.0000 -150.0000 106

 15 omega   34.00   63.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -30.0000  -30.0000 29

 16 omega   40.00  122.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027 -125.0000  -60.0000 82

 17 omega   12.00  115.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5337   57.0000   30.0000 103

 18 omega   12.00  115.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5337   57.0000 -180.0000 103

 19 omega   12.00  115.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5337   57.0000   90.0000 103

 20 omega   77.00  158.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027   61.0000   90.0000 81

 21 omega   77.00  158.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027   30.0000    0.0000 81

 22 omega   74.00  158.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027   77.0000  -90.0000 84

 23 omega   74.00  158.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027   77.0000 -180.0000 84

 24 omega   74.00  158.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027   77.0000    0.0000 84

 25 omega   23.00   77.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -94.0000  -90.0000 54

 26 omega   80.00  158.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      107.4027   45.0000   60.0000 78
;
_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      0.1025284000
_diffrn_orient_matrix_UB_12      0.0581794000
_diffrn_orient_matrix_UB_13      0.0101023000
_diffrn_orient_matrix_UB_21      0.0224587000
_diffrn_orient_matrix_UB_22      0.0001453000
_diffrn_orient_matrix_UB_23      0.0856298000
_diffrn_orient_matrix_UB_31      0.0456934000
_diffrn_orient_matrix_UB_32      -0.0850416000
_diffrn_orient_matrix_UB_33      -0.0134927000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41052
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.822
_diffrn_reflns_theta_min         4.230
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.047
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   gaussian
_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)
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            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.2769
_exptl_crystal_size_mid          0.1201
_exptl_crystal_size_min          0.0779
_refine_diff_density_max         1.371
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     929
_refine_ls_number_reflns         14686
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0940P)^2^+3.2586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13355
_reflns_number_total             14686
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02896_si_002.cif
_cod_data_source_block           compound_2
_cod_original_cell_volume        3760.32(15)
_cod_original_formula_sum        'C92 H94 Br2 Co2 O0.50'
_cod_database_code               4347222
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C45 H45 Co Br'
_reflns_odcompleteness_completeness 99.26
_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 C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 O1-C91 \\sim O1-C94
 with sigma of 0.02
 C93-C94 \\sim C92-C93 \\sim C91-C92
 with sigma of 0.02
 C82-C81 \\sim C82-C81A \\sim C81-C78 \\sim C81A-C78
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim C91 \\sim C92 \\sim C93 \\sim C94: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01
Br1A \\sim Br1: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
C26 \\sim C26A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C81A \\sim C81: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(C73) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C81A(0.87) H81a(0.87) H81b(0.87) H25a(0.71) H25b(0.71) H25c(0.29)
 H25d(0.29) H82a(0.87) H82b(0.87) H82c(0.87) H82d(0.13) H82e(0.13) H82f(0.13)
 C26(0.71) H26a(0.71) H26b(0.71) H26c(0.71) Br1(0.75) O1(0.5) C94(0.5)
 H94a(0.5) H94b(0.5) C93(0.5) H93a(0.5) H93b(0.5) C92(0.5) H92a(0.5) H92b(0.5)
 C91(0.5) H91a(0.5) H91b(0.5) C26A(0.29) H26d(0.29) H26e(0.29) H26f(0.29)
 C81(0.13) H81c(0.13) H81d(0.13) Br1A(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C65(H65a,H65b), C89(H89a,H89b), C33(H33a,H33b), C41(H41a,H41b), C17(H17a,
 H17b), C81A(H81a,H81b), C25(H25a,H25b), C25(H25c,H25d), C57(H57a,H57b),
 C73(H73a,H73b), C49(H49a,H49b), C94(H94a,H94b), C93(H93a,H93b), C92(H92a,H92b),
  C91(H91a,H91b), C81(H81c,H81d)
5.b Me refined with riding coordinates:
 C82(H82a,H82b,H82c), C82(H82d,H82e,H82f)
5.c Aromatic/amide H refined with riding coordinates:
 C85(H85), C64(H64), C40(H40), C53(H53), C20(H20), C55(H55), C72(H72),
 C84(H84), C24(H24), C87(H87), C52(H52), C48(H48), C44(H44), C63(H63), C28(H28),
  C36(H36), C69(H69), C31(H31), C45(H45), C16(H16), C32(H32), C23(H23),
 C77(H77), C61(H61), C56(H56), C21(H21), C60(H60), C88(H88), C76(H76), C47(H47),
  C71(H71), C15(H15), C80(H80), C79(H79), C29(H29), C37(H37), C39(H39),
 C13(H13), C68(H68), C12(H12)
5.d Idealised Me refined as rotating group:
 C18(H18a,H18b,H18c), C42(H42a,H42b,H42c), C34(H34a,H34b,H34c), C26(H26a,H26b,
 H26c), C66(H66a,H66b,H66c), C58(H58a,H58b,H58c), C90(H90a,H90b,H90c), C50(H50a,
 H50b,H50c), C74(H74a,H74b,H74c), C26A(H26d,H26e,H26f)
;
_shelx_res_checksum              4223
_shelx_hkl_checksum              71444
_olex2_submission_special_instructions 'No special instructions were received'