Structural phase transitions in tetra(isopropylammonium) decachlorotricadmate(II), [(CH~3~)~2~CHNH~3~]~4~Cd~3~Cl~10~, crystal with a two-dimensional cadmium(II) halide network
Gagor, Anna; Waśkowska, Alicja; Czapla, Zbigniew; Dacko, Slawomir; Acta Crystallographica Section B 67 (2011) 122–129; doi:10.1107/S0108768110054583

data_2104941
_publ_section_title
;
 Structural phase transitions in tetra(isopropylammonium)
 decachlorotricadmate(II), [(CH~3~)~2~CHNH~3~]~4~Cd~3~Cl~10~, crystal
 with a two-dimensional cadmium(II) halide network
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              122
_journal_page_last               129
_journal_paper_doi               10.1107/S0108768110054583
_journal_volume                  67
_journal_year                    2011
_chemical_formula_sum            'C12 H40 Cd3 Cl10 N4'
_chemical_formula_weight         932.18
_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                   7.4298(5)
_cell_length_b                   22.0791(5)
_cell_length_c                   19.4442(6)
_cell_measurement_reflns_used    3010
_cell_measurement_temperature    320(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.79
_cell_volume                     3189.7(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      320(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'KUMA KM4-CCD'
_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  0.0297
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26736
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    2.829
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.49
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.6 (release 21-05-2007 CrysAlis171 .NET)
(compiled May 21 2007,16:32:00)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorles
_exptl_crystal_density_diffrn    1.941
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.495
_refine_ls_extinction_coef       0.00290(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         3010
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0615
_reflns_number_gt                2449
_reflns_number_total             3010
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            kd5047.cif
_cod_data_source_block           pbca
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               2104941
_cod_database_fobs_code          2104941