Synthetic [NiFe] Models with a Fluxional CO ligand
Chu, Xiaoxiao; Yu, Xin; Raje, Sakthi; Angamuthu, Raja; Ma, Jian-ping; Tung, Chen-Ho; Wang, Wenguang; Dalton Trans.  (2017) –; doi:10.1039/C7DT02892J

data_7044243
_publ_section_title
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 Synthetic [NiFe] Models with a Fluxional CO ligand
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02892J
_journal_year                    2017
_chemical_formula_moiety         'C44 H45 Fe Ni O P2 S2, B F4, C H2 Cl2'
_chemical_formula_sum            'C45 H47 B Cl2 F4 Fe Ni O P2 S2'
_chemical_formula_weight         1002.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
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_audit_update_record
;
2017-08-04 deposited with the CCDC.
2017-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                75.1978(9)
_cell_angle_beta                 75.7266(9)
_cell_angle_gamma                70.1808(9)
_cell_formula_units_Z            2
_cell_length_a                   12.4756(13)
_cell_length_b                   13.5051(14)
_cell_length_c                   14.9627(15)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.625
_cell_measurement_theta_min      2.365
_cell_volume                     2257.2(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'BRUKE APEXII'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32572
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         27.642
_diffrn_reflns_theta_min         1.761
_exptl_absorpt_coefficient_mu    1.071
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6348
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0626 before and 0.0384 after correction.
The Ratio of minimum to maximum transmission is 0.8514.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         10460
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0393P)^2^+3.1979P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0997
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8205
_reflns_number_total             10460
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02892j2.cif
_cod_data_source_block           p-1
_cod_database_code               7044243
_shelx_shelxl_version_number     2014/7
_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.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C75(H75A,H75B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C20(H20), C21(H21), C22(H22), C23(H23),
 C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C34(H34),
  C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              12408
_olex2_submission_special_instructions 'No special instructions were received'