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_4347223
_publ_section_title
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 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         'C45 H45 Br0.99 Ni'
_chemical_formula_sum            'C45 H45 Br0.99 Ni'
_chemical_formula_weight         723.63
_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             2015-10-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                93.205(4)
_cell_angle_beta                 115.813(4)
_cell_angle_gamma                116.063(4)
_cell_formula_units_Z            2
_cell_length_a                   12.3278(6)
_cell_length_b                   14.0042(6)
_cell_length_c                   14.1264(6)
_cell_measurement_reflns_used    8291
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.0210
_cell_measurement_theta_min      4.1430
_cell_volume                     1877.8(2)
_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    'ShelXT (Sheldrick, 2015)'
_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 0.967
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_details
;
  1 omega  -97.00   -5.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      -41.0337  125.0000  150.0000 92

  2 omega  -66.00   30.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      -41.0337   37.0000  150.0000 96

  3 omega   26.00   92.00   1.0000    4.0900
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -94.0000  150.0000 66

  4 omega   31.00   94.00   1.0000    4.0900
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -94.0000    0.0000 63

  5 omega   80.00  156.00   1.0000    4.0900
omega____ theta____ kappa____ phi______ frames
    -      107.4027   77.0000  -90.0000 76

  6 omega   82.00  157.00   1.0000    4.0900
omega____ theta____ kappa____ phi______ frames
    -      107.4027   77.0000   30.0000 75

  7 omega   33.00   68.00   1.0000    4.0900
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -45.0000  -30.0000 35

  8 omega   36.00  109.00   1.0000    4.0900
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -94.0000  -90.0000 73

  9 omega   80.00  144.00   1.0000    4.0900
omega____ theta____ kappa____ phi______ frames
    -      107.4027   45.0000   90.0000 64

 10 omega -117.00  -15.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      -41.0337  -37.0000  150.0000 102

 11 omega -115.00  -11.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      -41.0337  -57.0000    0.0000 104

 12 omega   46.00  158.00   1.0000    4.0900
omega____ theta____ kappa____ phi______ frames
    -      107.4027   15.0000 -120.0000 112

 13 omega   74.00  158.00   1.0000    4.0900
omega____ theta____ kappa____ phi______ frames
    -      107.4027   77.0000  -30.0000 84

 14 omega   33.00   77.00   1.0000    4.0900
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -45.0000   30.0000 44

 15 omega   30.00   69.00   1.0000    4.0900
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -30.0000 -120.0000 39

 16 omega -120.00   -7.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      -41.0337  -77.0000  120.0000 113

 17 omega -115.00  -11.00   1.0000    1.0200
omega____ theta____ kappa____ phi______ frames
    -      -41.0337  -57.0000  -90.0000 104

 18 omega   77.00  158.00   1.0000    4.0900
omega____ theta____ kappa____ phi______ frames
    -      107.4027   61.0000  120.0000 81

 19 omega   23.00   48.00   1.0000    4.0900
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -94.0000   60.0000 25

 20 omega   23.00  109.00   1.0000    4.0900
omega____ theta____ kappa____ phi______ frames
    -      107.4027  -94.0000 -150.0000 86
;
_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      -0.0393335000
_diffrn_orient_matrix_UB_12      0.0608503000
_diffrn_orient_matrix_UB_13      0.0618451000
_diffrn_orient_matrix_UB_21      0.1495719000
_diffrn_orient_matrix_UB_22      0.0560363000
_diffrn_orient_matrix_UB_23      0.1015845000
_diffrn_orient_matrix_UB_31      0.0483759000
_diffrn_orient_matrix_UB_32      0.0984865000
_diffrn_orient_matrix_UB_33      -0.0452135000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16116
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         73.715
_diffrn_reflns_theta_min         4.188
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.185
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91831
_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            'dark red brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       block
_exptl_crystal_F_000             755
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7054
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0794P)^2^+1.0121P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1381
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6314
_reflns_number_total             7054
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02896_si_002.cif
_cod_data_source_block           compound_3
_cod_original_cell_volume        1877.78(17)
_cod_database_code               4347223
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C45H45NiBr
_reflns_odcompleteness_completeness 96.45
_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
Br1A \\sim Br1B \\sim Br1: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
3. Others
 Fixed Sof: H28a(0.6) H28b(0.6) H28c(0.4) H28d(0.4) Br1A(0.48143) C29(0.6)
 H29a(0.6) H29b(0.6) H29c(0.6) Br1B(0.23483) C29A(0.4) H29d(0.4) H29e(0.4)
 H29f(0.4) Br1(0.27408)
4.a Secondary CH2 refined with riding coordinates:
 C28(H28a,H28b), C28(H28c,H28d), C20(H20a,H20b), C12(H12a,H12b), C2AA(H2Aa,
 H2Ab), C1(H1a,H1b)
4.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C40(H40), C43(H43), C32(H32), C34(H34), C31(H31), C27(H27),
 C24(H24), C23(H23), C8(H8), C19(H19), C15(H15), C42(H42), C16(H16), C35(H35),
 C11(H11), C39(H39), C18(H18), C26(H26), C7(H7)
4.c Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C21(H21a,H21b,H21c), C29(H29a,H29b,H29c), C29A(H29d,H29e,
 H29f), C3AA(H3Aa,H3Ab,H3Ac), C4AA(H4Aa,H4Ab,H4Ac)
;
_shelx_res_checksum              60557
_shelx_hkl_checksum              92407
_olex2_submission_special_instructions 'No special instructions were received'