Synthesis and structure of pseudo-three dimensional hybrid iodobismuthate semiconductors.
Dennington, Adam J.; Weller, Mark T.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 17974–17979; doi:10.1039/c6dt03602c

data_7040974
_publ_section_title
;
 Synthesis and structure of pseudo-three dimensional hybrid iodobismuthate
 semiconductors.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17974
_journal_page_last               17979
_journal_paper_doi               10.1039/c6dt03602c
_journal_volume                  45
_journal_year                    2016
_chemical_formula_iupac          '[CH3NH(CH2)4NH2][BiI4]2.3H2O'
_chemical_formula_moiety         'Bi2 I8, (C5 N2 H14), 3(H2O)'
_chemical_formula_sum            'C5 H20 Bi2 I8 N2 O3'
_chemical_formula_weight         1589.2696
_chemical_name_systematic
'1-Methyl-1,4-Dipiperazinium iodobismuthate trihydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_audit_creation_date             2016-09-12
_audit_creation_method           'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_audit_update_record
;
2016-10-14 deposited with the CCDC.
2016-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.481(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6488(4)
_cell_length_b                   13.1532(8)
_cell_length_c                   13.7033(7)
_cell_measurement_reflns_used    3426
_cell_measurement_temperature    292.23(10)
_cell_measurement_theta_max      31.0430
_cell_measurement_theta_min      4.0740
_cell_volume                     1369.83(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics
'Palmer, D. C. (2014). CrystalMaker. CrystalMaker Software Ltd, Begbroke, Oxfordshire, England.'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.23(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9975
_diffrn_measured_fraction_theta_max 0.8819
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w    -51.00 -10.00   1.00   15.00    --  -22.90 -38.00 150.00   41
  2  \w    -80.00  -1.00   1.00   15.00    --  -22.90 -77.00 120.00   79
  3  \w      8.00  93.00   1.00   15.00    --   23.69  38.00  30.00   85
  4  \w     25.00  63.00   1.00   15.00    --   23.69 -99.00 -90.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0033010000
_diffrn_orient_matrix_UB_12      -0.0397127000
_diffrn_orient_matrix_UB_13      -0.0347416000
_diffrn_orient_matrix_UB_21      0.0034315000
_diffrn_orient_matrix_UB_22      -0.0364058000
_diffrn_orient_matrix_UB_23      0.0383656000
_diffrn_orient_matrix_UB_31      -0.0932134000
_diffrn_orient_matrix_UB_32      -0.0027985000
_diffrn_orient_matrix_UB_33      -0.0057488000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8333
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        29.5096
_diffrn_reflns_theta_max         32.0057
_diffrn_reflns_theta_min         3.3042
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    43.639
_exptl_absorpt_correction_T_max  0.040
_exptl_absorpt_correction_T_min  0.006
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    3.804
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.176
_refine_diff_density_max         1.431
_refine_diff_density_min         -2.822
_refine_diff_density_rms         0.416
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         4206
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3350
_reflns_number_total             4206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03602c2.cif
_cod_data_source_block           Compound2_RT
_cod_depositor_comments
'Adding full bibliography for 7040972--7040977.cif.'
_cod_database_code               7040974
_cell_oxdiff_length_a            7.6492(3)
_cell_oxdiff_length_b            13.1480(9)
_cell_oxdiff_length_c            13.7094(7)
_cell_oxdiff_angle_alpha         89.974(5)
_cell_oxdiff_angle_beta          96.531(4)
_cell_oxdiff_angle_gamma         90.058(4)
_cell_oxdiff_volume              1369.82(13)
_cell_oxdiff_measurement_reflns_used 3426
_oxdiff_exptl_absorpt_empirical_full_min 0.636
_oxdiff_exptl_absorpt_empirical_full_max 1.554
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_theta     29.51
_reflns_odcompleteness_iscentric 1
_shelx_res_checksum              79942