Three- and Four-Coordinate Homoleptic Iron(I)‒NHC Complexes: Synthesis and Characterization
Ouyang, Zhenwu; Meng, Yinshan; Cheng, Jun; Xiao, Jie; Gao, Song; Deng, Liang; Organometallics 35 (2016) 1361–; doi:10.1021/acs.organomet.6b00047

data_4088385
_publ_section_title
;
 Three- and Four-Coordinate Homoleptic Iron(I)--NHC Complexes: Synthesis
 and Characterization
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1361
_journal_paper_doi               10.1021/acs.organomet.6b00047
_journal_volume                  35
_journal_year                    2016
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C33 H60 Fe N6, C24 H20 B'
_chemical_formula_sum            'C57 H80 B Fe N6'
_chemical_formula_weight         915.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.032(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1175(9)
_cell_length_b                   15.8118(14)
_cell_length_c                   17.1337(16)
_cell_measurement_reflns_used    4871
_cell_measurement_temperature    130
_cell_measurement_theta_max      23.09
_cell_measurement_theta_min      2.45
_cell_volume                     2647.2(4)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0874
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27209
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.231
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0705 before and 0.0527 after correction.
The Ratio of minimum to maximum transmission is 0.8605.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       block
_exptl_crystal_F_000             990
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.949
_refine_diff_density_min         -1.275
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         10313
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0754
_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^)+(0.1139P)^2^+2.6887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1913
_refine_ls_wR_factor_ref         0.2101
_reflns_Friedel_coverage         0.926
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                8178
_reflns_number_total             10313
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00047_si_002.cif
_cod_data_source_block           5
_cod_database_code               4088385
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.908
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C31 \\sim C32 \\sim C33: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
C8 \\sim C9 \\sim C10 \\sim N1: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C9) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C8(H8), C11(H11), C18(H18), C21(H21), C28(H28), C31(H31)
3.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C42(H42),
 C43(H43), C44(H44), C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51),
  C53(H53), C54(H54), C55(H55), C56(H56), C57(H57)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              24429
_shelx_hkl_checksum              1177
_olex2_submission_special_instructions 'No special instructions were received'