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_4347221
_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         'C90 H90 Br2 Fe2, C7 H8'
_chemical_formula_sum            'C97 H98 Br2 Fe2'
_chemical_formula_weight         1535.27
_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
_atom_sites_solution_primary     direct
_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                92.656(4)
_cell_angle_beta                 114.368(4)
_cell_angle_gamma                116.014(5)
_cell_formula_units_Z            1
_cell_length_a                   12.4894(5)
_cell_length_b                   13.9380(8)
_cell_length_c                   14.1966(6)
_cell_measurement_reflns_used    9659
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      28.3790
_cell_measurement_theta_min      3.5990
_cell_volume                     1943.5(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 7.9851
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_details
;
  1 omega  -89.00    0.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4258  -57.0000   60.0000 89

  2 omega  -81.00  -43.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4258  132.0000  152.7391 38

  3 omega  -87.00   12.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4258  -77.0000  -60.0000 99

  4 omega  -82.00   17.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4258  -19.0000  120.0000 99

  5 omega   35.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1133  178.0000 -150.0000 62

  6 omega  -13.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1133   77.0000 -120.0000 103

  7 omega   35.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1133  178.0000    0.0000 62

  8 omega  -98.00  -34.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4258  178.0000  -90.0000 64

  9 omega  -92.00    8.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4258  -38.0000   90.0000 100

 10 omega  -41.00   50.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.4258   57.0000 -150.0000 91

 11 omega  -20.00    5.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.1133  -99.0000   90.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0641922000
_diffrn_orient_matrix_UB_12      0.0121294000
_diffrn_orient_matrix_UB_13      0.0058486000
_diffrn_orient_matrix_UB_21      -0.0106216000
_diffrn_orient_matrix_UB_22      -0.0514235000
_diffrn_orient_matrix_UB_23      0.0114747000
_diffrn_orient_matrix_UB_31      -0.0311498000
_diffrn_orient_matrix_UB_32      -0.0261327000
_diffrn_orient_matrix_UB_33      -0.0556224000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.898
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32419
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.996
_diffrn_reflns_theta_min         3.327
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.449
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.814
_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 red'
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             802
_exptl_crystal_size_max          0.1929
_exptl_crystal_size_mid          0.1124
_exptl_crystal_size_min          0.0619
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         9269
_refine_ls_number_restraints     288
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+1.8441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7161
_reflns_number_total             9269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02896_si_002.cif
_cod_data_source_block           compound_1b
_cod_original_cell_volume        1943.52(18)
_cod_database_code               4347221
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C97H98Br2Fe2
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2. Uiso/Uaniso restraints and constraints
C00E \\sim C00U \\sim C00R \\sim C4 \\sim C10 \\sim C11: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.02
C017 \\sim C01C \\sim C019 \\sim C018 \\sim C3 \\sim C0 \\sim C01D \\sim C12
\\sim C3A \\sim C13: within 2A with sigma of 0.02 and sigma for terminal atoms
of 0.02
C8 \\sim C7 \\sim C1 \\sim C5 \\sim C2: within 5A with sigma of 0.02 and sigma
for terminal atoms of 0.02
Br1 \\sim Br2 \\sim Br3 \\sim Br4: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.02
Uanis(C00E) = Uanis(C00U) = Uanis(C00R) = Uanis(C4) = Uanis(C10) = Uanis(C11)
3. Others
 Fixed Sof: Br2(0.39) C00E(0.5) C00U(0.5) H00U(0.5) C017(0.5) H017(0.5)
 C01C(0.5) C019(0.5) H019(0.5) C00R(0.5) H00R(0.5) C018(0.5) H01l(0.5)
 H01m(0.5) H01n(0.5) Br3(0.25) C3(0.5) H3a(0.5) H3b(0.5) C2(0.5) C5(0.5)
 H5(0.5) C9(0.5) H9(0.5) C1(0.5) H1(0.5) C7(0.5) H7(0.5) C8(0.5) H8(0.5)
 C6(0.5) H6a(0.5) H6b(0.5) H6c(0.5) Br4(0.13) Br1(0.23) C4(0.5) C10(0.5)
 H10(0.5) C0(0.5) H0(0.5) C01D(0.5) C12(0.5) H12(0.5) C11(0.5) H11(0.5)
 C3A(0.5) H3Aa(0.5) H3Ab(0.5) C13(0.5) H13a(0.5) H13b(0.5) H13c(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C00X(H00i,H00j), C00Y(H00k,H00m), C00Z(H00s,H00v), C013(H01a,H01b), C3(H3a,
 H3b), C3A(H3Aa,H3Ab)
4.b Aromatic/amide H refined with riding coordinates:
 C003(H003), C008(H008), C00B(H00B), C00D(H00D), C00U(H00U), C017(H017),
 C019(H019), C00R(H00R), C00F(H00F), C00G(H00G), C00H(H00H), C00L(H00L),
 C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q), C00T(H00T), C00W(H00W),
 C010(H010), C011(H011), C5(H5), C9(H9), C1(H1), C7(H7), C8(H8), C10(H10),
 C0(H0), C12(H12), C11(H11)
4.c Fitted hexagon refined as free rotating group:
 C00E(C00U,C017,C01C,C019,C00R), C4(C10,C0,C01D,C12,C11)
4.d Idealised Me refined as rotating group:
 C00S(H00a,H00c,H00e), C014(H01c,H01d,H01e), C015(H01f,H01g,H01h), C016(H01i,
 H01j,H01k), C018(H01l,H01m,H01n), C6(H6a,H6b,H6c), C13(H13a,H13b,H13c)
;
_shelx_res_checksum              7127
_shelx_hkl_checksum              38139
_olex2_submission_special_instructions 'No special instructions were received'