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_7044247
_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      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-04-15
_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                90.00
_cell_angle_beta                 95.945(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.869(10)
_cell_length_b                   18.068(12)
_cell_length_c                   15.881(11)
_cell_measurement_reflns_used    2830
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.824
_cell_measurement_theta_min      2.347
_cell_volume                     3958(5)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER APEXII'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71000
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_unetI/netI     0.0834
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22914
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.85
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.079
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0696 before and 0.0542 after correction.
The Ratio of minimum to maximum transmission is 0.8694.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       solid
_exptl_crystal_F_000             1800
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         6991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+4.3590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                4542
_reflns_number_total             6991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt02892j2.cif
_cod_data_source_block           p_CCDC3
_cod_database_code               7044247
_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:
 C2(H2A,H2B), C16(H16A,H16B), C1(H1A,H1B), C3(H3A,H3B), C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C30(H30), C21(H21), C17(H17), C33(H33), C34(H34), C20(H20),
 C28(H28), C37(H37), C31(H31), C24(H24), C32(H32), C27(H27), C40(H40), C38(H38),
  C26(H26), C19(H19), C39(H39), C18(H18), C25(H25)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C13(H13A,H13B,
 H13C), C12(H12A,H12B,H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'