Synthesis, structural, characterization and Hirshfeld analysis of a bisselenide and a zinc complex of a new hemilabile ferrocenylbisphosphane, [Fe{C~5~H~4~P(C~6~H~4~CH~2~NMe~2~-<i>o</i>)~2~}~2~]
Kunchur, Harish S.; Mondal, Dipanjan; Rao, Sowmya; Mague, Joel T.; Balakrishna, Maravanji S.; Acta Crystallographica Section C 77 (2021) 725–733; doi:10.1107/S205322962101072X

data_2022576
_publ_section_title
;
 Synthesis, structural, characterization and Hirshfeld analysis of a
 bisselenide and a zinc complex of a new hemilabile
 ferrocenylbisphosphane,
 [Fe{C~5~H~4~P(C~6~H~4~CH~2~NMe~2~-<i>o</i>)~2~}~2~]
;
_journal_coeditor_code           ZO3012
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              725
_journal_page_last               733
_journal_paper_doi               10.1107/S205322962101072X
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[Fe Zn2 Cl4 (C23 H28 N2 P1)2], C H2 Cl2'
_chemical_formula_moiety         'C46 H56 Cl4 Fe N4 P2 Zn2, C H2 Cl2'
_chemical_formula_sum            'C47 H58 Cl6 Fe N4 P2 Zn2'
_chemical_formula_weight         1140.20
_chemical_name_systematic
;[\m-1,1'-Bis(bis{2-[(dimethylamino)methyl]phenyl}phosphanyl)ferrocene-\k^2^<i>N</i>,<i>P</i>:\k^2^<i>N</i>',<i>P</i>']bis[dichloridozinc(II)]
dichloromethane monosolvate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                96.791(2)
_cell_angle_beta                 91.486(2)
_cell_angle_gamma                116.491(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1150(13)
_cell_length_b                   10.7515(14)
_cell_length_c                   26.637(3)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.7324
_cell_measurement_theta_min      2.3191
_cell_volume                     2564.4(6)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_data_collection
;
<i>APEX3</i> (Bruker, 2016)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Brandenburg & Putz, 2012)
;
_computing_publication_material
;
<i>SHELXTL</i> (Bruker, 2016)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3660
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.0927
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            48081
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         28.738
_diffrn_reflns_theta_min         2.139
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.619
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>TWINABS</i>; Sheldrick, 2009)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.039
_refine_diff_density_min         -0.633
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         48081
_refine_ls_number_restraints     294
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0197P)^2^+4.4933P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1277
_reflns_number_gt                41125
_reflns_number_total             48081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zo3012sup1.cif
_cod_data_source_block           Compound_3
_cod_database_code               2022576
_shelx_estimated_absorpt_t_min   0.759
_shelx_estimated_absorpt_t_max   0.961
_shelx_hkl_checksum              30423
_shelx_res_checksum              53039
_cod_database_fobs_code 2022576