Stepwise assembly of heterobimetallic complexes: synthesis, structure, and physical properties.
Lee, Justin L.; Oswald, Victoria F.; Biswas, Saborni; Hill, Ethan A.; Ziller, Joseph W.; Hendrich, Michael P.; Borovik, A. S.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 8111–8119; doi:10.1039/d1dt01021b

data_7707435
_publ_section_title
;
 Stepwise assembly of heterobimetallic complexes: synthesis, structure,
 and physical properties.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8111
_journal_page_last               8119
_journal_paper_doi               10.1039/d1dt01021b
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_sum            'C52 H64 F3 Fe N7 Ni O7 P3 S'
_chemical_formula_weight         1195.63
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-03-23 deposited with the CCDC.	2021-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.3910(9)
_cell_length_b                   17.3399(8)
_cell_length_c                   29.1742(13)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      28.67
_cell_measurement_theta_min      2.34
_cell_volume                     10821.2(8)
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1046
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            152061
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.720
_diffrn_reflns_theta_min         1.396
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             4984
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane, methylene chloride'
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.086
_refine_diff_density_max         1.056
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.245(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1356
_refine_ls_number_reflns         27950
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+8.3974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0988
_reflns_Friedel_coverage         0.962
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                21063
_reflns_number_total             27950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01021b2.cif
_cod_data_source_block           asb621
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not_measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7707432--7707435.cif.
;
_cod_database_code               7707435
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.818
_shelx_estimated_absorpt_t_max   0.933
_exptl_absorpt_special_details
; 
Reflections not merged 
156938 Corrected reflections written to file asb621s.hkl 
Estimated minimum and maximum transmission:  0.6779  0.7458 
The ratio(0.9090) of these values is more reliable than their absolute values 
Additional spherical absorption correction applied with mu*r =  0.2000 
Lambda/2 correction factor = 0.00150 
;
_shelx_res_checksum              558