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_4347224
_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         'C110 H130 Br2 Ni2'
_chemical_formula_sum            'C110 H130 Br2 Ni2'
_chemical_formula_weight         1729.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-03-11
_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                 90.0983(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.41135(16)
_cell_length_b                   22.5367(3)
_cell_length_c                   31.9869(4)
_cell_measurement_reflns_used    22425
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.9440
_cell_measurement_theta_min      3.5360
_cell_volume                     9667.9(2)
_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)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
  1 omega  -47.00  -20.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -44.0756   38.0000 -180.0000 27

  2 omega  -59.00    1.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -44.0756   57.0000   30.0000 60

  3 omega  -72.00   29.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -44.0756   19.0000  -60.0000 101

  4 omega   63.00   91.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000   60.0000 28

  5 omega   43.00  120.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000  150.0000 77

  6 omega   67.00   98.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000 -150.0000 31

  7 omega   32.00   88.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  -60.0000 56

  8 omega   33.00   65.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  120.0000 32

  9 omega   46.00  113.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -61.0000  120.0000 67

 10 omega   35.00   68.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  -90.0000 33

 11 omega   53.00   98.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000 -180.0000 45

 12 omega   47.00  133.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000  -30.0000 86

 13 omega   14.00  116.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       44.3256   77.0000 -120.0000 102

 14 omega   20.00  107.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       44.3256   57.0000    0.0000 87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0183794000
_diffrn_orient_matrix_UB_12      -0.0126122000
_diffrn_orient_matrix_UB_13      0.0467063000
_diffrn_orient_matrix_UB_21      -0.0617189000
_diffrn_orient_matrix_UB_22      -0.0552587000
_diffrn_orient_matrix_UB_23      -0.0116927000
_diffrn_orient_matrix_UB_31      0.0950461000
_diffrn_orient_matrix_UB_32      -0.0382574000
_diffrn_orient_matrix_UB_33      0.0014987000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            51679
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.224
_diffrn_reflns_theta_min         2.763
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.783
_exptl_absorpt_correction_T_max  0.883
_exptl_absorpt_correction_T_min  0.761
_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            'reddish brown'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       block
_exptl_crystal_F_000             3664
_exptl_crystal_size_max          0.2415
_exptl_crystal_size_mid          0.1549
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1123
_refine_ls_number_reflns         19083
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0648P)^2^+3.1380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1237
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16030
_reflns_number_total             19083
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02896_si_002.cif
_cod_data_source_block           compound_4
_cod_original_cell_volume        9667.94(19)
_cod_database_code               4347224
_chemical_oxdiff_formula         C110H130Ni2Br2
_chemical_oxdiff_usercomment     'red plate'
_reflns_odcompleteness_completeness 99.74
_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
 H53D-H55E
 2.01 with sigma of 0.001
3. Others
 Fixed Sof: H99A(0.65) H99B(0.65) H99C(0.35) H99D(0.35) C52(0.8) H52A(0.8)
 H52B(0.8) H54A(0.8) H54B(0.8) H54C(0.2) H54D(0.2) H42A(0.8) H42B(0.8)
 H42C(0.2) H42D(0.2) C53(0.8) H53A(0.8) H53B(0.8) H55A(0.8) H55B(0.8) H55C(0.8)
 H55D(0.2) H55E(0.2) H55F(0.2) H13A(0.7) H13B(0.7) H13C(0.3) H13D(0.3)
 H68A(0.52) H68B(0.52) H68C(0.48) H68D(0.48) H10C(0.65) H10D(0.65) H10E(0.65)
 H10F(0.35) H10G(0.35) H10H(0.35) C43(0.8) H43A(0.8) H43B(0.8) C100(0.65)
 H10I(0.65) H10J(0.65) C14(0.7) H14A(0.7) H14B(0.7) C101(0.65) H10K(0.65)
 H10L(0.65) C44(0.8) H44A(0.8) H44B(0.8) C69(0.52) H69A(0.52) H69B(0.52)
 C70(0.52) H70A(0.52) H70B(0.52) H70C(0.52) C45(0.8) H45A(0.8) H45B(0.8)
 H45C(0.8) C15(0.7) H15A(0.7) H15B(0.7) H15C(0.7) C72(0.48) H72A(0.48)
 H72B(0.48) H72C(0.48) C71(0.48) H71A(0.48) H71B(0.48) C14A(0.3) H14C(0.3)
 H14D(0.3) C1A(0.35) H1AA(0.35) H1AB(0.35) C1B(0.35) H1BA(0.35) H1BB(0.35)
 C15A(0.3) H15D(0.3) H15E(0.3) H15F(0.3) C52A(0.2) H52C(0.2) H52D(0.2)
 C53A(0.2) H53C(0.2) H53D(0.2) C44A(0.2) H44C(0.2) H44D(0.2) C43A(0.2)
 H43C(0.2) H43D(0.2) C0AA(0.2) H0AA(0.2) H0AB(0.2) H0AC(0.2)
4.a Secondary CH2 refined with riding coordinates:
 C90(H90A,H90B), C91(H91A,H91B), C33(H33A,H33B), C89(H89A,H89B), C32(H32A,
 H32B), C34(H34A,H34B), C109(H10A,H10B), C99(H99A,H99B), C99(H99C,H99D),
 C12(H12A,H12B), C110(H11A,H11B), C67(H67A,H67B), C22(H22A,H22B), C52(H52A,
 H52B), C54(H54A,H54B), C54(H54C,H54D), C79(H79A,H79B), C111(H11C,H11D),
 C42(H42A,H42B), C42(H42C,H42D), C24(H24A,H24B), C23(H23A,H23B), C80(H80A,H80B),
  C53(H53A,H53B), C13(H13A,H13B), C13(H13C,H13D), C81(H81A,H81B), C68(H68A,
 H68B), C68(H68C,H68D), C43(H43A,H43B), C100(H10I,H10J), C14(H14A,H14B),
 C101(H10K,H10L), C44(H44A,H44B), C69(H69A,H69B), C71(H71A,H71B), C14A(H14C,
 H14D), C1A(H1AA,H1AB), C1B(H1BA,H1BB), C52A(H52C,H52D), C53A(H53C,H53D),
 C44A(H44C,H44D), C43A(H43C,H43D)
4.b Me refined with riding coordinates:
 C102(H10C,H10D,H10E), C102(H10F,H10G,H10H)
4.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C10(H10), C7(H7), C104(H104), C28(H28), C84(H84), C94(H94),
 C37(H37), C88(H88), C87(H87), C11(H11), C8(H8), C62(H62), C74(H74), C47(H47),
 C31(H31), C78(H78), C63(H63), C41(H41), C85(H85), C97(H97), C17(H17), C98(H98),
  C95(H95), C105(H105), C75(H75), C20(H20), C66(H66), C38(H38), C18(H18),
 C48(H48), C108(H108), C30(H30), C21(H21), C40(H40), C51(H51), C77(H77),
 C50(H50), C65(H65), C107(H107)
4.d Idealised Me refined as rotating group:
 C92(H92A,H92B,H92C), C25(H25A,H25B,H25C), C35(H35A,H35B,H35C), C55(H55A,H55B,
 H55C), C55(H55D,H55E,H55F), C82(H82A,H82B,H82C), C112(H11E,H11F,H11G),
 C70(H70A,H70B,H70C), C45(H45A,H45B,H45C), C15(H15A,H15B,H15C), C72(H72A,H72B,
 H72C), C15A(H15D,H15E,H15F), C0AA(H0AA,H0AB,H0AC)
;
_shelx_res_checksum              15058
_shelx_hkl_checksum              94581
_shelx_fab_checksum              52814
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'CryoStream 700, Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder with inert oil'
_olex2_submission_special_instructions 'No special instructions were received'