Crystal structure of bis[(<i>R</i>,<i>R</i>)-1,2-(binaphthylphosphonito)ethane]dichloridoiron(II) dichloromethane disolvate
Rennie, Benjamin E.; Lough, Alan J.; Morris, Robert H.; Acta Crystallographica Section E 76 (2020) 1525–1527; doi:10.1107/S2056989020011160

data_2243569
_publ_section_title
;
 Crystal structure of
 bis[(<i>R</i>,<i>R</i>)-1,2-(binaphthylphosphonito)ethane]dichloridoiron(II)
 dichloromethane disolvate
;
_journal_coeditor_code           HB7939
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1525
_journal_page_last               1527
_journal_paper_doi               10.1107/S2056989020011160
_journal_volume                  76
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_iupac          '[Fe Cl2 (C42 H28 O4 P2)2], 2C H2 Cl2'
_chemical_formula_moiety         'C84 H56 Cl2 Fe O8 P4, 2(C H2 Cl2)'
_chemical_formula_sum            'C86 H60 Cl6 Fe O8 P4'
_chemical_formula_weight         1613.77
_chemical_name_common
;
Bis[(<i>R</i>,<i>R</i>)-1,2-(binaphthylphosphonito)ethane]dichloridoiron(II)
dichloromethane disolvate
;
_chemical_name_systematic
'Bis{1,2-bis[12,14-dioxa-13-phosphapentacyclo[13.8.0.0^2,11^.0^3,8^.0^18,23^]tricosa-1(15),2(11),3(8),4,6,9,16,18(23),19,21-decaen-13-yl]ethane}dichloridoiron(II) dichloromethane disolvate'
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                   11.9850(3)
_cell_length_b                   11.9850(3)
_cell_length_c                   52.4508(14)
_cell_measurement_reflns_used    6128
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      67.28
_cell_measurement_theta_min      3.37
_cell_volume                     7534.0(3)
_computing_cell_refinement
;
APEX3 (Bruker, 2018)
;
_computing_data_collection
;
APEX3 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1091
_diffrn_reflns_av_unetI/netI     0.0628
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            97444
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.792
_diffrn_reflns_theta_min         3.370
_diffrn_source                   'Bruker ImuS with multi-layer optics'
_exptl_absorpt_coefficient_mu    4.840
_exptl_absorpt_correction_T_max  0.7395
_exptl_absorpt_correction_T_min  0.6486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       Shard
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.651
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2237 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.004(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         6829
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+2.6304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                6096
_reflns_number_total             6829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb7939sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        7534.0(4)
_cod_database_code               2243569
_shelx_estimated_absorpt_t_min   0.670
_shelx_estimated_absorpt_t_max   0.909
_shelx_hkl_checksum              23908
_shelx_res_checksum              12766
_cod_database_fobs_code 2243569