Investigation of iron-ammine and amido complexes within a C<sub>3</sub>-symmetrical phosphinic amido tripodal ligand.
Sun, Chen; Oswald, Victoria F.; Hill, Ethan A.; Ziller, Joseph W.; Borovik, A. S.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 11197–11205; doi:10.1039/d1dt01032h

data_7707869
_publ_section_title
;
 Investigation of iron-ammine and amido complexes within a
 C<sub>3</sub>-symmetrical phosphinic amido tripodal ligand.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11197
_journal_page_last               11205
_journal_paper_doi               10.1039/d1dt01032h
_journal_volume                  50
_journal_year                    2021
_chemical_formula_sum            'C96 H108 Fe2 K2 N8 O9 P6'
_chemical_formula_weight         1893.62
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-01-02 deposited with the CCDC.	2021-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   14.8465(13)
_cell_length_b                   14.8465(13)
_cell_length_c                   85.868(8)
_cell_measurement_reflns_used    6757
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      22.93
_cell_measurement_theta_min      2.47
_cell_volume                     16391(3)
_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      133(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0855
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       109
_diffrn_reflns_limit_l_min       -109
_diffrn_reflns_number            44415
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         27.116
_diffrn_reflns_theta_min         1.423
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.482
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       prism
_exptl_crystal_F_000             5952
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuran, diethyl ether'
_exptl_crystal_size_max          0.543
_exptl_crystal_size_mid          0.385
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         4029
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0429P)^2^+58.1010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1256
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2771
_reflns_number_total             4029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01032h2.cif
_cod_data_source_block           asb542_sq
_cod_depositor_comments
'Adding full bibliography for 7707868--7707872.cif.'
_cod_database_code               7707869
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.780
_shelx_estimated_absorpt_t_max   0.889
_exptl_absorpt_special_details
; 
 Reflections not merged 
   47374 Corrected reflections written to file asb542s.hkl 
 Estimated minimum and maximum transmission:  0.6822  0.7455 
 The ratio(0.9151) 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              543
_shelx_fab_checksum              64152