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_1558995
_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_absolute_configuration ad
_chemical_formula_moiety         'C72 H86 Fe N6 P4, 2(B F4), 2(C2 H3 N)'
_chemical_formula_sum            'C76 H92 B2 F8 Fe N8 P4'
_chemical_formula_weight         1470.92
_chemical_melting_point          413
_chemical_name_systematic
;
[Bis(3,7-dibenzyl-1,5-di(1&#x0092;-(R)-phenylethyl)-1,5-diaza-3,7-diphosphacyclooctane)-
bis(acetonitrile)iron(II)] tetrafluoroborate
;
_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   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7178(14)
_cell_length_b                   20.452(2)
_cell_length_c                   27.659(3)
_cell_measurement_reflns_used    2995
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.24
_cell_measurement_theta_min      2.35
_cell_volume                     7759.9(14)
_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      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_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  0.1968
_diffrn_reflns_av_unetI/netI     0.1829
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            134467
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.842
_diffrn_reflns_theta_min         2.842
_exptl_absorpt_coefficient_mu    0.342
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6194
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       plate
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 2312 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     866
_refine_ls_number_reflns         14690
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.2051
_refine_ls_R_factor_gt           0.0791
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+10.3179P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.2081
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.846
_reflns_number_gt                7289
_reflns_number_total             14690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            complex_8_rev.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        7759.8(14)
_cod_database_code               1558995
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              18802
_shelx_hkl_checksum              64362