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_7707871
_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            'C62 H85 Cl4 Fe K N7 O9 P3'
_chemical_formula_weight         1402.03
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-01-02 deposited with the CCDC.	2021-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                101.9506(7)
_cell_angle_beta                 98.9294(7)
_cell_angle_gamma                118.7866(7)
_cell_formula_units_Z            2
_cell_length_a                   14.6635(7)
_cell_length_b                   14.8610(7)
_cell_length_c                   18.8343(9)
_cell_measurement_reflns_used    9861
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      28.74
_cell_measurement_theta_min      2.32
_cell_volume                     3360.0(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 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.0177
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39019
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         1.157
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.8015
_exptl_absorpt_correction_T_min  0.7193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             1472
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, pentane'
_exptl_crystal_size_max          0.393
_exptl_crystal_size_mid          0.391
_exptl_crystal_size_min          0.178
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     804
_refine_ls_number_reflns         14722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0430P)^2^+3.1983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13000
_reflns_number_total             14722
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01032h2.cif
_cod_data_source_block           asb550
_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 7707868--7707872.cif.
;
_cod_original_cell_volume        3359.9(3)
_cod_database_code               7707871
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.805
_shelx_estimated_absorpt_t_max   0.904
_exptl_absorpt_special_details
; 
 Reflections not merged 
   40636 Corrected reflections written to file asb550s.hkl 
 Estimated minimum and maximum transmission:  0.7193  0.8015 
 The ratio (0.8974) of these values is more reliable than their absolute values! 
 Additional spherical absorption correction applied with mu*r =  0.1500 
 Lambda/2 correction factor = 0.00150 
;
_shelx_res_checksum              16305