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_4347225
_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         'C55 H65 Co I2'
_chemical_formula_sum            'C55 H65 Co I2'
_chemical_formula_weight         1038.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-19
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.501(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1662(5)
_cell_length_b                   25.8886(9)
_cell_length_c                   13.6321(4)
_cell_measurement_reflns_used    9568
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      74.1580
_cell_measurement_theta_min      3.5980
_cell_volume                     4881.0(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
  1 omega  -22.00   66.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0756  -57.0000  -60.0000 176

  2 omega   20.00  109.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0756   57.0000   90.0000 178

  3 omega   32.00   91.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000   90.0000 118

  4 omega   44.00   81.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000 -150.0000 74

  5 omega   69.00  106.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000 -120.0000 74

  6 omega   81.00  169.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  125.0000 -120.0000 176

  7 omega   38.00  105.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000    0.0000 134

  8 omega   32.00   86.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  150.0000 108

  9 omega   20.00  113.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0756   57.0000  -90.0000 186

 10 omega   20.00   33.50   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0756   57.0000    0.0000 27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0100464000
_diffrn_orient_matrix_UB_12      -0.0590170000
_diffrn_orient_matrix_UB_13      0.0134839000
_diffrn_orient_matrix_UB_21      0.0080091000
_diffrn_orient_matrix_UB_22      -0.0055073000
_diffrn_orient_matrix_UB_23      -0.1103306000
_diffrn_orient_matrix_UB_31      0.1106518000
_diffrn_orient_matrix_UB_32      0.0057522000
_diffrn_orient_matrix_UB_33      0.0320772000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19921
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.422
_diffrn_reflns_theta_min         3.195
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.931
_exptl_absorpt_correction_T_max  0.797
_exptl_absorpt_correction_T_min  0.267
_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            'dark brown'
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.1516
_exptl_crystal_size_mid          0.0411
_exptl_crystal_size_min          0.018
_refine_diff_density_max         2.376
_refine_diff_density_min         -1.528
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         9494
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0798P)^2^+5.6902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8001
_reflns_number_total             9494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02896_si_002.cif
_cod_data_source_block           compound_5
_cod_database_code               4347225
_chemical_oxdiff_formula         C55H65CoI2
_chemical_oxdiff_usercomment     'red rod'
_reflns_odcompleteness_completeness 99.14
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C16-C15 \\sim C15-C14
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C12 \\sim C13 \\sim C15 \\sim C14 \\sim C18 \\sim C17 \\sim C16: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C12(0.67) H12A(0.67) H12B(0.67) C13(0.67) H13A(0.67) H13B(0.67)
 H15A(0.67) H15B(0.67) H15C(0.67) H15D(0.33) H15E(0.33) H15F(0.33) C14(0.67)
 H14A(0.67) H14B(0.67) C18(0.33) H18A(0.33) H18B(0.33) C17(0.33) H17A(0.33)
 H17B(0.33) C16(0.33) H16A(0.33) H16B(0.33)
5.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C35(H35A,H35B), C55(H55A,H55B), C36(H36A,
 H36B), C25(H25A,H25B), C37(H37A,H37B), C45(H45A,H45B), C46(H46A,H46B),
 C56(H56A,H56B), C57(H57A,H57B), C47(H47A,H47B), C26(H26A,H26B), C27(H27A,H27B),
  C14(H14A,H14B), C18(H18A,H18B), C17(H17A,H17B), C16(H16A,H16B)
5.b Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C15(H15D,H15E,H15F)
5.c Aromatic/amide H refined with riding coordinates:
 C31(H31), C7(H7), C20(H20), C30(H30), C34(H34), C40(H40), C11(H11), C44(H44),
 C24(H24), C53(H53), C21(H21), C50(H50), C43(H43), C54(H54), C8(H8), C33(H33),
 C51(H51), C41(H41), C23(H23), C10(H10)
5.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C58(H58A,H58B,H58C), C48(H48A,H48B,H48C), C28(H28A,H28B,
 H28C)
;
_shelx_res_checksum              98611
_shelx_hkl_checksum              1756
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'