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_7707868
_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            'C44 H49 Fe N5 O3.5 P3'
_chemical_formula_weight         852.64
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      trigonal
_space_group_IT_number           143
_space_group_name_Hall           'P 3'
_space_group_name_H-M_alt        'P 3'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   17.2520(6)
_cell_length_b                   17.2520(6)
_cell_length_c                   8.2626(3)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      29.04
_cell_measurement_theta_min      2.36
_cell_volume                     2129.74(13)
_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      88(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.954
_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  0.0152
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            26581
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.147
_diffrn_reflns_theta_min         1.363
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  0.8016
_exptl_absorpt_correction_T_min  0.7752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             894
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, pentane'
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.254
_exptl_crystal_size_min          0.222
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
; 
 Flack x determined using 3370 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.002(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         7144
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0237
_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^)+(0.0379P)^2^+0.6678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0630
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.899
_reflns_number_gt                7061
_reflns_number_total             7144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01032h2.cif
_cod_data_source_block           asb551
_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        2129.74(17)
_cod_original_formula_sum        'C44 H49 Fe N5 O3.50 P3'
_cod_database_code               7707868
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.858
_shelx_estimated_absorpt_t_max   0.895
_exptl_absorpt_special_details
; 
Reflections not merged 
26581 Corrected reflections written to file asb551s.hkl 
Estimated minimum and maximum transmission:  0.7752  0.8016 
The ratio (0.9671) 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              71175