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_7707872
_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_absolute_configuration ad
_chemical_formula_sum            'C49 H49 Fe K N5 O3 P3'
_chemical_formula_weight         943.79
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     'dual space'
_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                90
_cell_formula_units_Z            4
_cell_length_a                   14.8454(10)
_cell_length_b                   17.4775(11)
_cell_length_c                   19.4608(13)
_cell_measurement_reflns_used    9530
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.10
_cell_measurement_theta_min      2.33
_cell_volume                     5049.3(6)
_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 0.993
_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  0.0502
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            61149
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.306
_diffrn_reflns_theta_min         1.566
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       prism
_exptl_crystal_F_000             1968
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, pentane'
_exptl_crystal_size_max          0.323
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.186
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.011(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     550
_refine_ls_number_reflns         12304
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0430P)^2^+2.3859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.0994
_reflns_Friedel_coverage         0.826
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                10451
_reflns_number_total             12304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01032h2.cif
_cod_data_source_block           asb583_sq
_cod_depositor_comments
'Adding full bibliography for 7707868--7707872.cif.'
_cod_database_code               7707872
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.850
_shelx_estimated_absorpt_t_max   0.910
_exptl_absorpt_special_details
; 
Reflections not merged 
   61273 Corrected reflections written to file asb583s.hkl 
 Estimated minimum and maximum transmission:  0.6837  0.7457 
 The ratio (0.9169) 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              52291
_shelx_fab_checksum              79215