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_4347226
_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 I2 Ni'
_chemical_formula_sum            'C55 H65 I2 Ni'
_chemical_formula_weight         1038.58
_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                 102.5499(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.11866(12)
_cell_length_b                   25.8867(2)
_cell_length_c                   13.67535(12)
_cell_measurement_reflns_used    27197
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      74.2360
_cell_measurement_theta_min      3.6010
_cell_volume                     4878.72(7)
_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 10.3546
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
  1 omega  -64.00   33.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9564   37.0000  150.0000 194

  2 omega   18.00  116.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9564   37.0000    0.0000 196

  3 omega   48.00  122.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300 -125.0000  150.0000 148

  4 omega   34.00   64.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300  -30.0000 -150.0000 60

  5 omega   41.00   77.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300  -45.0000 -180.0000 72

  6 omega   33.00  108.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300  -94.0000  -30.0000 150

  7 omega   42.00   69.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300  -30.0000 -120.0000 54

  8 omega   79.00  157.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300   61.0000   30.0000 156

  9 omega   74.00  158.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300  125.0000  -90.0000 168

 10 omega  -67.00   35.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9564   37.0000  -60.0000 204

 11 omega -115.00  -11.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9564  -57.0000  150.0000 208

 12 omega  -69.00   -5.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000   30.0000   90.0000 128

 13 omega   78.00  158.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300   30.0000  150.0000 160

 14 omega   30.00   69.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300  -30.0000  120.0000 78

 15 omega   78.00  158.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300   61.0000 -120.0000 160

 16 omega -115.00  -11.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9564  -57.0000   30.0000 208

 17 omega -120.00   -7.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9564  -77.0000  -90.0000 226

 18 omega   78.00  158.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300   30.0000  -30.0000 160

 19 omega   81.00  158.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300   45.0000   90.0000 154

 20 omega   24.00  109.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300  -94.0000 -150.0000 170

 21 omega   78.00  158.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      108.2300   61.0000 -180.0000 160

 22 omega -120.00  -95.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9564  -77.0000    0.0000 50

 23 omega    2.00   98.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9564 -125.0000   30.0000 192
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0396953000
_diffrn_orient_matrix_UB_12      0.0464176000
_diffrn_orient_matrix_UB_13      -0.0491143000
_diffrn_orient_matrix_UB_21      0.1011468000
_diffrn_orient_matrix_UB_22      -0.0088213000
_diffrn_orient_matrix_UB_23      0.0676192000
_diffrn_orient_matrix_UB_31      0.0262829000
_diffrn_orient_matrix_UB_32      -0.0362210000
_diffrn_orient_matrix_UB_33      -0.0795147000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            47011
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         74.441
_diffrn_reflns_theta_min         3.207
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.753
_exptl_absorpt_correction_T_max  0.703
_exptl_absorpt_correction_T_min  0.085
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_description       needle
_exptl_crystal_F_000             2116
_exptl_crystal_size_max          0.6828
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.0498
_refine_diff_density_max         1.185
_refine_diff_density_min         -1.174
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         9776
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+2.0188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9245
_reflns_number_total             9776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02896_si_002.cif
_cod_data_source_block           compound_6
_cod_original_cell_volume        4878.71(7)
_cod_database_code               4347226
_chemical_oxdiff_formula         'C55 H65 Ni I2'
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C9 \\sim C16 \\sim C12 \\sim C15 \\sim C13 \\sim C14 \\sim C17: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: H14A(0.64) H14B(0.64) H14C(0.36) H14D(0.36) C12(0.64) H12A(0.64)
 H12B(0.64) C13(0.64) H13A(0.64) H13B(0.64) C16(0.36) H16A(0.36) H16B(0.36)
 C15(0.36) H15A(0.36) H15B(0.36)
4.a Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B), C24(H24A,H24B), C34(H34A,H34B), C35(H35A,H35B), C44(H44A,
 H44B), C56(H56A,H56B), C36(H36A,H36B), C55(H55A,H55B), C25(H25A,H25B),
 C45(H45A,H45B), C46(H46A,H46B), C26(H26A,H26B), C14(H14A,H14B), C14(H14C,H14D),
  C12(H12A,H12B), C13(H13A,H13B), C16(H16A,H16B), C15(H15A,H15B)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C29(H29), C33(H33), C32(H32), C39(H39), C11(H11), C20(H20), C42(H42),
 C22(H22), C49(H49), C43(H43), C19(H19), C53(H53), C23(H23), C52(H52), C30(H30),
  C8(H8), C50(H50), C40(H40), C10(H10)
4.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C57(H57A,H57B,H57C), C47(H47A,H47B,H47C), C17(H17A,H17B,
 H17C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              49708
_shelx_hkl_checksum              93008
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'