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_7044244
_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, 2(B F4)'
_chemical_formula_sum            'C44 H42 B2 F8 Fe Ni O P2 S2'
_chemical_formula_weight         1001.01
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_date             2017-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-10 deposited with the CCDC.
2017-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.973(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9924(4)
_cell_length_b                   15.2087(4)
_cell_length_c                   28.0744(12)
_cell_measurement_reflns_used    4662
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.5520
_cell_measurement_theta_min      4.3030
_cell_volume                     4675.8(3)
_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 0.993
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'BRUKER APEXII'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0819
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            17804
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.806
_diffrn_reflns_theta_min         3.160
_exptl_absorpt_coefficient_mu    5.031
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       solid
_exptl_crystal_F_000             2048
_refine_diff_density_max         1.995
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         8780
_refine_ls_number_restraints     73
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1724
_refine_ls_R_factor_gt           0.1362
_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^)+(0.1158P)^2^+95.5171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3272
_refine_ls_wR_factor_ref         0.3509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6155
_reflns_number_total             8780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02892j2.cif
_cod_data_source_block           p
_cod_database_code               7044244
_shelxl_version_number           2013-4
_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. Restrained distances
 C43-C58
 1.55 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C4 \\sim C5 \\sim C6 \\sim C1 \\sim C2 \\sim C3: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
C8 \\sim C7 \\sim C9 \\sim C10 \\sim C11 \\sim C12: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.08
4.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11), C12(H12), C7(H7), C8(H8),
 C14(H14), C15(H15), C16(H16), C17(H17), C13(H13), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30)
4.c Fitted hexagon refined as free rotating group:
 C9(C10,C11,C12,C7,C8), C14(C15,C16,C17,C18,C13)
4.d Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              5762
_shelx_fab_checksum              36433
_olex2_submission_special_instructions 'No special instructions were received'