Synthesis, characterization and disorder‒order phase transition of inorganic‒organic hybrid materials (H2dabco-CH2-Cl)[MIICl4] (M = Co, Zn)
Chen, Chun-Hong; Xu, Guan-Cheng; CrystEngComm 18 (2016) 550–; doi:10.1039/C5CE02059J

data_7223409
_publ_section_title
;
 Synthesis, characterization and disorder--order phase transition of
 inorganic--organic hybrid materials (H2dabco-CH2-Cl)[MIICl4] (M = Co, Zn)
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              550
_journal_paper_doi               10.1039/C5CE02059J
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C7 H15 Cl5 N2 Zn'
_chemical_formula_weight         369.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-12-02 deposited with the CCDC.
2015-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.190(6)
_cell_length_b                   10.204(6)
_cell_length_c                   12.278(7)
_cell_measurement_reflns_used    3971
_cell_measurement_temperature    363(2)
_cell_measurement_theta_max      25.8192
_cell_measurement_theta_min      2.4626
_cell_volume                     1401.9(14)
_computing_cell_refinement       'Bruker SMART APEX II'
_computing_data_collection       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      363(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9844
_diffrn_reflns_theta_full        25.09
_diffrn_reflns_theta_max         25.09
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    2.676
_exptl_absorpt_correction_T_max  0.5108
_exptl_absorpt_correction_T_min  0.4814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0061(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         1326
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+1.6816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0669
_reflns_number_gt                1193
_reflns_number_total             1326
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce02059j2.cif
_cod_data_source_block           Zn363K
_cod_depositor_comments
'Adding full bibliography for 7223407--7223410.cif.'
_cod_original_cell_volume        1402.0(13)
_cod_original_sg_symbol_H-M      Pnma
_cod_original_formula_sum        'C7 H15 Cl5 N2  Zn'
_cod_database_code               7223409