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_7040975
_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         1589.4214
_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                 96.347(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5434(2)
_cell_length_b                   13.0515(5)
_cell_length_c                   13.6716(5)
_cell_measurement_reflns_used    7248
_cell_measurement_temperature    149.95(10)
_cell_measurement_theta_max      32.0140
_cell_measurement_theta_min      4.1080
_cell_volume                     1337.76(8)
_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      N~2~
_diffrn_ambient_temperature      149.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9974
_diffrn_measured_fraction_theta_max 0.8963
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w     63.00  89.00   1.00   15.00    --   22.86  77.00 -60.00   26
  2  \w     -4.00  86.00   1.00   15.00    --   22.86  77.00 150.00   90
  3  \w    -31.00  87.00   1.00   15.00    --   22.86   0.00 150.00  118
  4  \w    -18.00  62.00   1.00   15.00    --   22.86 -99.00   0.00   80
  5  \w     23.00  76.00   1.00   15.00    --   22.86-125.00 -68.00   53
  6  \w    -68.00 -26.00   1.00   15.00    --  -22.08 125.00   9.00   42
;
_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      0.0080410000
_diffrn_orient_matrix_UB_12      -0.0274125000
_diffrn_orient_matrix_UB_13      0.0450972000
_diffrn_orient_matrix_UB_21      -0.0209936000
_diffrn_orient_matrix_UB_22      -0.0461741000
_diffrn_orient_matrix_UB_23      -0.0260658000
_diffrn_orient_matrix_UB_31      0.0918855000
_diffrn_orient_matrix_UB_32      -0.0081400000
_diffrn_orient_matrix_UB_33      -0.0039772000
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14198
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        29.5096
_diffrn_reflns_theta_max         32.0964
_diffrn_reflns_theta_min         3.3418
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    22.371
_exptl_absorpt_correction_T_max  0.055
_exptl_absorpt_correction_T_min  0.007
_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    7.890
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2538.000
_exptl_crystal_size_max          0.434
_exptl_crystal_size_mid          0.189
_exptl_crystal_size_min          0.168
_refine_diff_density_max         1.841
_refine_diff_density_min         -2.820
_refine_diff_density_rms         0.382
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         4214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0275P)^2^+2.7875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3779
_reflns_number_total             4214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03602c2.cif
_cod_data_source_block           Compound2_150K
_cod_depositor_comments
'Adding full bibliography for 7040972--7040977.cif.'
_cod_database_code               7040975
_cell_oxdiff_length_a            7.5441(2)
_cell_oxdiff_length_b            13.0598(5)
_cell_oxdiff_length_c            13.6609(5)
_cell_oxdiff_angle_alpha         89.993(3)
_cell_oxdiff_angle_beta          96.325(3)
_cell_oxdiff_angle_gamma         90.012(3)
_cell_oxdiff_volume              1337.75(8)
_cell_oxdiff_measurement_reflns_used 7248
_oxdiff_exptl_absorpt_empirical_full_min 0.747
_oxdiff_exptl_absorpt_empirical_full_max 1.424
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_theta     29.51
_reflns_odcompleteness_iscentric 1
_shelx_res_checksum              91954