Crystal structure of bis{(<i>S</i>)-1-[2-(diphenylphosphanyl)ferrocenyl]-(<i>R</i>)-ethyl}ammonium bromide dichloromethane monosolvate
Zirakzadeh, Afrooz; Stöger, Berthold; Kirchner, Karl; Acta Crystallographica Section E 73 (2017) 152–154; doi:10.1107/S2056989016020417

data_2242011
_publ_section_title
;
 Crystal structure of
 bis{(<i>S</i>)-1-[2-(diphenylphosphanyl)ferrocenyl]-(<i>R</i>)-ethyl}ammonium
 bromide dichloromethane monosolvate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              152
_journal_page_last               154
_journal_paper_doi               10.1107/S2056989016020417
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Fe2 (C5 H5)2 (C38 H36 N P2)] Br, C H2 Cl2'
_chemical_formula_moiety         'C48 H46 Fe2 N P2 +, Br -, C H2 Cl2'
_chemical_formula_sum            'C49 H48 Br Cl2 Fe2 N P2'
_chemical_formula_weight         975.33
_chemical_name_systematic
;Bis{(<i>S</i>)-1-[2-(diphenylphosphanyl)ferrocenyl]-(<i>R</i>)-ethyl}ammonium
bromide dichloromethane monosolvate
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           78
_space_group_name_Hall           'P 4cw'
_space_group_name_H-M_alt        'P 43'
_symmetry_space_group_name_Hall  'P 4cw'
_symmetry_space_group_name_H-M   'P 43'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2463(7)
_cell_length_b                   11.2463(7)
_cell_length_c                   33.938(2)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.64
_cell_measurement_theta_min      2.17
_cell_volume                     4292.5(5)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2015)
;
_computing_data_collection
;
APEX2 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2015)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\w- and \f-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            42331
_diffrn_reflns_theta_full        30.012
_diffrn_reflns_theta_max         30.012
_diffrn_reflns_theta_min         2.172
_exptl_absorpt_coefficient_mu    1.842
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2015)
;
_exptl_crystal_colour            'translucent yellow'
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       tabular
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.852
_refine_diff_density_min         -0.411
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 4530 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.002(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         12559
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0324
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0078P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0625
_reflns_number_gt                10851
_reflns_number_total             12559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2595sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        4292.5(6)
_cod_database_code               2242011
_shelx_estimated_absorpt_t_min   0.565
_shelx_estimated_absorpt_t_max   0.823
_shelx_hkl_checksum              78175
_shelx_res_checksum              10405
_cod_database_fobs_code 2242011