Synthesis and Structure of Iron (II) Complexes of Functionalized 1,5-Diaza-3,7-Diphosphacyclooctanes.
Spiridonova, Yulia S.; Nikolaeva, Yulia A.; Balueva, Anna S.; Musina, Elvira I.; Litvinov, Igor A.; Strelnik, Igor D.; Khrizanforova, Vera V.; Budnikova, Yulia G.; Karasik, Andrey A.; Molecules (Basel, Switzerland) 25 (2020) 3775–; doi:10.3390/molecules25173775

data_1558996
_publ_section_title
;
 Synthesis and Structure of Iron (II) Complexes of Functionalized
 1,5-Diaza-3,7-Diphosphacyclooctanes.
;
_journal_issue                   17
_journal_name_full               'Molecules (Basel, Switzerland)'
_journal_page_first              3775
_journal_paper_doi               10.3390/molecules25173775
_journal_volume                  25
_journal_year                    2020
_chemical_formula_moiety
'3(C68 H68 B F4 Fe N4 P4), 2(B F4), 15(C3 H6 O), [+ solvent]'
_chemical_formula_sum            'C249 H294 B5 F20 Fe3 N12 O15 P12'
_chemical_formula_weight         4704.49
_chemical_melting_point          413
_chemical_name_systematic
;
[Bis(3,7-dibenzyl-1,5-di(1?-(R)-phenylethyl)-1,5-diaza-3,7-diphosphacyclooctane)-
tetrafluoroboratoiron(II)] tetrafluoroborate
;
_space_group_crystal_system      trigonal
_space_group_IT_number           150
_space_group_name_Hall           'P 3 2"'
_space_group_name_H-M_alt        'P 3 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   22.651(2)
_cell_length_b                   22.651(2)
_cell_length_c                   15.3431(17)
_cell_measurement_reflns_used    1008
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.64
_cell_measurement_theta_min      2.23
_cell_volume                     6817.4(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker 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  0.2490
_diffrn_reflns_av_unetI/netI     0.2653
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            29199
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.685
_exptl_absorpt_coefficient_mu    0.297
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4675
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 1062 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         8934
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.2191
_refine_ls_R_factor_gt           0.1040
_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^)+(0.1253P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2221
_refine_ls_wR_factor_ref         0.2794
_reflns_Friedel_coverage         0.853
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4109
_reflns_number_total             8934
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            complex11b-resub.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        6817.3(16)
_cod_database_code               1558996
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.943
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              35078
_shelx_hkl_checksum              14360
_shelx_fab_checksum              47763