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_7044246
_publ_section_title
;
 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'
_chemical_formula_sum            'C44 H45 B F4 Fe Ni O P2 S2'
_chemical_formula_weight         917.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-08-04 deposited with the CCDC.
2017-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.322(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.394(3)
_cell_length_b                   13.100(2)
_cell_length_c                   25.930(4)
_cell_measurement_reflns_used    4184
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.184
_cell_measurement_theta_min      2.257
_cell_volume                     5018.3(15)
_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)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'BRUKE APEXII'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_unetI/netI     0.1087
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            29118
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.076
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1149 before and 0.0634 after correction.
The Ratio of minimum to maximum transmission is 0.7106.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_platon_squeeze_details
;
;
_refine_diff_density_max         2.409
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         8842
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0702
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1070P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1759
_refine_ls_wR_factor_ref         0.1948
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5400
_reflns_number_total             8842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02892j2.cif
_cod_data_source_block           p_CCDC2
_cod_original_cell_volume        5018.2(15)
_cod_database_code               7044246
_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. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F4: within 1.7A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C19(H19), C21(H21), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C33(H33),
  C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              38983
_olex2_submission_special_instructions 'No special instructions were received'