Bis(tetrabutylammonium) tetrachloridomanganate(II) dichloromethane disolvate
Hay, Michael T.; Yennawar, Hemant P.; IUCrData 8 (2023) x230610–; doi:10.1107/S2414314623006107

data_1569535
_publ_section_title
;
 Bis(tetrabutylammonium) tetrachloridomanganate(II) dichloromethane
 disolvate
;
_journal_coeditor_code           WM4191
_journal_issue                   7
_journal_name_full               IUCrData
_journal_page_first              x230610
_journal_paper_doi               10.1107/S2414314623006107
_journal_volume                  8
_journal_year                    2023
_chemical_formula_iupac          '(C16 H36 N)2 [Mn Cl4], 2C H2 Cl2'
_chemical_formula_moiety         '2(C16 H36 N +), Mn Cl4 2-, 2(C H2 Cl2)'
_chemical_formula_sum            'C34 H76 Cl8 Mn N2'
_chemical_formula_weight         851.50
_chemical_name_systematic
;
Bis(tetrabutylammonium) tetrachloridomanganate(II) dichloromethane disolvate
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0775(3)
_cell_length_b                   14.0775(3)
_cell_length_c                   24.3492(8)
_cell_measurement_reflns_used    3369
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      60.7560
_cell_measurement_theta_min      3.6160
_cell_volume                     4825.4(2)
_computing_cell_refinement
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_collection
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku OD, 2021)
;
_computing_molecular_graphics
;
Olex2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
Olex2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
<i>olex2.solve</i> (Bourhis <i>et al.</i>,  2015)
;
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            9265
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.135
_diffrn_reflns_theta_min         3.627
_diffrn_source                   'Rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    6.463
_exptl_absorpt_correction_T_max  0.359
_exptl_absorpt_correction_T_min  0.060
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(<i>CrysAlisPro</i>; Rigaku OD, 2021)
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       plate
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.350
_refine_diff_density_min         -0.317
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 458 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   -0.018(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         2334
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0754
_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^)+(0.1133P)^2^+4.1001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2016
_refine_ls_wR_factor_ref         0.2215
_reflns_number_gt                1567
_reflns_number_total             2334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm4191.cif
_cod_data_source_block           I
_cod_original_cell_volume        4825.4(3)
_cod_database_code               1569535
_shelx_estimated_absorpt_t_min   0.193
_shelx_estimated_absorpt_t_max   0.487