Bis(4-methylbenzylammonium) tetrachloridozincate: a new noncentrosymmetric structure characterized by ^13^C CP‒MAS NMR spectroscopy
Kefi, Riadh; Jeanneau, Erwann; Lefebvre, Frédéric; Ben Nasr, Cherif; Acta Crystallographica Section C 67 (2011) m126–m129; doi:10.1107/S0108270111012297

data_2018088
_publ_section_title
;
 Bis(4-methylbenzylammonium) tetrachloridozincate: a new
 noncentrosymmetric structure characterized by ^13^C CP--MAS NMR
 spectroscopy
;
_journal_coeditor_code           WQ3001
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m126
_journal_page_last               m129
_journal_paper_doi               10.1107/S0108270111012297
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C8 H12 N)2 [Zn Cl4]'
_chemical_formula_moiety         '2(C8 H12 N +), Cl4 Zn 2-'
_chemical_formula_sum            'C16 H24 Cl4 N2 Zn'
_chemical_formula_weight         451.57
_chemical_name_systematic
;
Bis(4-methylbenzylammonium) tetrachloridozincate
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6623(8)
_cell_length_b                   25.395(2)
_cell_length_c                   7.4167(5)
_cell_measurement_reflns_used    11472
_cell_measurement_temperature    110
_cell_measurement_theta_max      29.5605
_cell_measurement_theta_min      3.3393
_cell_volume                     2008.2(3)
_computing_cell_refinement       'CrysAlis PRO (Agilent Technologies, 2010)'
_computing_data_collection       'CrysAlis PRO (Agilent Technologies, 2010)'
_computing_data_reduction        'CrysAlis PRO (Agilent Technologies, 2010)'
_computing_molecular_graphics    'CAMERON (Watkin <i>et al.</i>, 1996)'
_computing_publication_material  'CRYSTALS (Betteridge <i>et al.</i>, 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>, 2003)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      110
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Make? Model? CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            26378
_diffrn_reflns_theta_full        27.551
_diffrn_reflns_theta_max         29.624
_diffrn_reflns_theta_min         3.441
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.755
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Agilent Technologies, 2010), based on expressions derived
by Clark & Reid (1995)]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.085
_refine_diff_density_max         1.10
_refine_diff_density_min         -1.36
_refine_ls_abs_structure_details
'Flack & Bernardinelli (1999), with 2877 Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_coef       40(5)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9240
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         5120
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.0000990
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982)
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
 A~i~ are:
 0.168E+04 0.269E+04 0.142E+04 428.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1430
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1430
_reflns_number_gt                4699
_reflns_number_total             5120
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wq3001.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C16 H24 Cl4 N2 Zn1'
_cod_database_code               2018088
_cod_database_fobs_code          2018088