[NH(2)(C(2)H(4))(2)O]MX(5): a new family of morpholinium nonlinear optical materials among halogenoantimonate(iii) and halogenobismuthate(iii) compounds. Structural characterization, dielectric and piezoelectric properties.
Owczarek, Magdalena; Szklarz, Przemysław; Jakubas, Ryszard; Miniewicz, Andrzej; Dalton transactions (Cambridge, England : 2003) 41 (2012) 7285–7294; doi:10.1039/c2dt30291h

data_7019397
_publ_section_title
;
 [NH(2)(C(2)H(4))(2)O]MX(5): a new family of morpholinium nonlinear
 optical materials among halogenoantimonate(iii) and
 halogenobismuthate(iii) compounds. Structural characterization,
 dielectric and piezoelectric properties.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7285
_journal_page_last               7294
_journal_paper_doi               10.1039/c2dt30291h
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'Bi Br5, 2(C4 H10 N O)'
_chemical_formula_sum            'C8 H20 Bi Br5 N2 O2'
_chemical_formula_weight         784.79
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   9.246(3)
_cell_length_b                   10.331(3)
_cell_length_c                   18.694(5)
_cell_measurement_reflns_used    13603
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.8
_cell_measurement_theta_min      2.9
_cell_volume                     1785.7(9)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.804
_diffrn_measurement_device_type
'Goniometer KM4/Xcalibur, detector: Sapphire2 (large Be window)'
_diffrn_measurement_method       \w
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0370
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            18664
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         36.91
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    21.059
_exptl_absorpt_correction_T_max  0.125
_exptl_absorpt_correction_T_min  0.020
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.32 (release 27-01-2009 CrysAlis171 .NET)
(compiled Jan 27 2009,14:17:37)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.919
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.555
_refine_diff_density_min         -1.195
_refine_diff_density_rms         0.169
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.042(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         6519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0159P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0367
_refine_ls_wR_factor_ref         0.0372
_reflns_number_gt                5840
_reflns_number_total             6519
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt30291h.txt
_cod_data_source_block           morbib
_cod_database_code               7019397