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_2104940
_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_coeditor_code           KD5047
_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           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m 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                   7.4634(2)
_cell_length_b                   22.0476(10)
_cell_length_c                   19.6139(9)
_cell_measurement_reflns_used    2337
_cell_measurement_temperature    375(2)
_cell_measurement_theta_max      29.76
_cell_measurement_theta_min      2.78
_cell_volume                     3227.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      375(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.942
_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  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            14304
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         29.76
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    2.79
_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    1.918
_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         0.349
_refine_diff_density_min         -0.406
_refine_ls_extinction_coef       0.00042(3)
_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   0.899
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         2333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0490
_refine_ls_wR_factor_ref         0.0539
_reflns_number_gt                1659
_reflns_number_total             2333
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            kd5047.cif
_cod_data_source_block           Cmce
_cod_original_sg_symbol_H-M      Cmce
_cod_database_code               2104940
_cod_database_fobs_code          2104940