Bis[<i>N</i>,<i>N</i>'-diisopropyl-<i>N</i>-(trimethylsilyl)benzamidinium] di-μ-chloro-bis[tetrachlorozirconate(IV)] dichloromethane disolvate
Roberto Centore; Angela Tuzi; Dario Liguori; Acta Crystallographica Section C 59 (2003) m241–m242; doi:10.1107/S0108270103010035

data_2013337
_publ_section_title
;
 Bis[<i>N</i>,<i>N</i>'-diisopropyl-<i>N</i>-(trimethylsilyl)benzamidinium]
 di-\m-chloro-bis[tetrachlorozirconate(IV)] dichloromethane disolvate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m241
_journal_page_last               m242
_journal_paper_doi               10.1107/S0108270103010035
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '(C16 H29 N2 Si)2 [Zr2 Cl10], 2C H2 Cl2'
_chemical_formula_moiety         '2C16 H29 N2 Si 1+, 2C1 H2 Cl2, Zr2 Cl10 2-'
_chemical_formula_structural
;
(C16 H29 N2 Si)2 (Zr2 Cl10) (C1 H2 Cl2)2
;
_chemical_formula_sum            'C34 H62 Cl14 N4 Si2 Zr2'
_chemical_formula_weight         1261.80
_chemical_name_systematic
;
Bis[N,N'-diisopropyl-N-(trimethylsilyl)benzamidinium]
di-\m-chloro-bis[tetrachlorozirconate(IV)] dichloromethane disolvate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.61(5)
_cell_length_b                   17.350(2)
_cell_length_c                   16.832(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.43
_cell_measurement_theta_min      28.23
_cell_volume                     5727(15)
_computing_cell_refinement       'CELLFIT (Centore, 2002)'
_computing_data_collection       'MACH3/PC & CAD4/PC (Nonius, 1996)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
;
WinGX publication routines (Farrugia, 1999)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius MACH3'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6872
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  126
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.087
_exptl_absorpt_correction_T_max  0.7214
_exptl_absorpt_correction_T_min  0.5029
_exptl_absorpt_correction_type   '\f scan'
_exptl_absorpt_process_details
;
North et al. (1968).
The number of psi-scan sets used was 3.
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.548
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         6872
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0624P)^2^+7.0008P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1469
_reflns_number_gt                4109
_reflns_number_total             6872
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na1614.cif
_cod_data_source_block           I
_cod_database_code               2013337
_cod_database_fobs_code          2013337