Crystal structure of bis(<i>N</i>-<i>tert</i>-butylbenzamidinium) hexachloridozirconate(IV) dichloromethane disolvate
Jiang, Zhi-Hao; Zhao, Jian-Ping; Ma, Xiu-Ming; Bai, Sheng-Di; Acta Crystallographica Section E 72 (2016) 432–435; doi:10.1107/S2056989016003030

data_2241587
_publ_section_title
;
 Crystal structure of bis(<i>N</i>-<i>tert</i>-butylbenzamidinium)
 hexachloridozirconate(IV) dichloromethane disolvate
;
_journal_coeditor_code           XU5884
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              432
_journal_page_last               435
_journal_paper_doi               10.1107/S2056989016003030
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '(C11 H17 N2) [Zr Cl6], 2C H2 Cl2'
_chemical_formula_moiety         '2(C11 H17 N2 +), Cl6 Zr 2-, 2(C H2 Cl2)'
_chemical_formula_sum            'C24 H38 Cl10 N4 Zr'
_chemical_formula_weight         828.30
_chemical_name_systematic
;
Bis(<i>N</i>-<i>tert</i>-butylbenzamidinium)
hexachloridozirconate(IV) dichloromethane disolvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.259(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.443(5)
_cell_length_b                   16.154(9)
_cell_length_c                   10.891(6)
_cell_measurement_reflns_used    2094
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21.945
_cell_measurement_theta_min      2.256
_cell_volume                     1836.8(17)
_computing_cell_refinement
;
SAINT (Bruker, 2000)
;
_computing_data_collection
;
SMART (Bruker, 2000)
;
_computing_data_reduction
;
SAINT (Bruker, 2000)
;
_computing_molecular_graphics
;
SHELXTL/PC (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART area-detector'
_diffrn_measurement_method       '\f and \w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0614
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10309
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    1.048
_exptl_absorpt_correction_T_max  0.8586
_exptl_absorpt_correction_T_min  0.8177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.731
_refine_diff_density_min         -0.897
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3410
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1176P)^2^+2.8350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1839
_refine_ls_wR_factor_ref         0.2132
_reflns_number_gt                2255
_reflns_number_total             3410
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            xu5884sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1836.9(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2241587
_cod_database_fobs_code 2241587