Investigation of structure-properties relationship in a novel family of halogenoantimonates(iii) and halogenobismuthates(iii) with morpholinium cation: [NH2(C2H4)2O]MX4. Crystal structure, phase transitions and dynamics of molecules.
Owczarek, Magdalena; Jakubas, Ryszard; Pietraszko, Adam; Medycki, Wojciech; Baran, Jan; Dalton transactions (Cambridge, England : 2003) 42 (2013) 15069–15079; doi:10.1039/c3dt51726h

data_7023661
_publ_section_title
;
 Investigation of structure-properties relationship in a novel family of
 halogenoantimonates(iii) and halogenobismuthates(iii) with morpholinium
 cation: [NH2(C2H4)2O]MX4. Crystal structure, phase transitions and
 dynamics of molecules.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15069
_journal_page_last               15079
_journal_paper_doi               10.1039/c3dt51726h
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C4 H10 Bi Br4 N O'
_chemical_formula_weight         616.75
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 108.33(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.666(3)
_cell_length_b                   12.675(3)
_cell_length_c                   8.0870(16)
_cell_measurement_temperature    300(2)
_cell_volume                     1232.4(5)
_computing_cell_refinement       'CRYSALIS V172.33.42'
_computing_data_collection       'CRYSALIS V172.33.42'
_computing_data_reduction        'CRYSALIS V172.33.42'
_computing_molecular_graphics    'DIAMOND 3.2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  KM4CCD
_diffrn_measurement_method       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  0.0538
_diffrn_reflns_av_sigmaI/netI    0.0753
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            14637
_diffrn_reflns_theta_full        29.63
_diffrn_reflns_theta_max         29.63
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    27.232
_exptl_absorpt_correction_T_max  1.4515
_exptl_absorpt_correction_T_min  0.5979
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CRYSALIS V172.33.42'
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    3.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       UNSHAPED
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.052
_refine_diff_density_min         -0.974
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       0.001403(11)
_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   0.819
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         3297
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.819
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+0.0150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0403
_refine_ls_wR_factor_ref         0.0426
_reflns_number_gt                2117
_reflns_number_total             3297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51726h.txt
_cod_data_source_block           p21c300
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'MONOCLINIC' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'NUMERICAL'
changed to 'numerical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1232.4(4)
_cod_original_sg_symbol_H-M      P2(1)/C
_cod_database_code               7023661