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_7044245
_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         'C40 H45 Fe Ni O P2 S2, B F4'
_chemical_formula_sum            'C40 H45 B F4 Fe Ni O P2 S2'
_chemical_formula_weight         869.19
_chemical_name_systematic
;
 ?
;
_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             2017-03-19
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-07-10 deposited with the CCDC.
2017-09-15 downloaded from the CCDC.
;
_cell_angle_alpha                80.1447(15)
_cell_angle_beta                 81.3355(15)
_cell_angle_gamma                69.6593(15)
_cell_formula_units_Z            2
_cell_length_a                   10.9679(19)
_cell_length_b                   13.573(2)
_cell_length_c                   16.458(3)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.483
_cell_measurement_theta_min      2.172
_cell_volume                     2252.3(7)
_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      173.15
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'BRUKER APEXII'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_number            7929
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.915
_exptl_absorpt_coefficient_mu    0.948
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6120
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0609 before and 0.0392 after correction.
The Ratio of minimum to maximum transmission is 0.8208.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       solid
_exptl_crystal_F_000             900
_platon_squeeze_details          'TITL p P -1 R = 0.11'
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0295P)^2^+2.6321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0886
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6755
_reflns_number_total             7929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02892j2.cif
_cod_data_source_block           p_CCDC1
_cod_original_cell_volume        2252.4(7)
_cod_database_code               7044245
_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. Others
 Fixed Sof: F0AA(0.6) F1AA(0.4) F3(0.4) F4(0.4) F5(0.6) F6(0.6)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C15(H15A,H15B), C16(H16A,H16B)
3.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
 C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34),
  C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,
 H8B,H8C)
;
_shelx_fab_checksum              43284
_olex2_submission_special_instructions 'No special instructions were received'