Synthesis and materials chemistry of bismuth tris-(di-i-propylcarbamate): deposition of photoactive Bi2O3 thin films.
Cosham, Samuel D.; Hill, Michael S.; Horley, Graeme A.; Johnson, Andrew L.; Jordan, Laura; Molloy, Kieran C.; Stanton, David C.; Inorganic chemistry 53 (2014) 503–511; doi:10.1021/ic402499r

data_4337478
_publ_section_title
;
 Synthesis and materials chemistry of bismuth tris-(di-i-propylcarbamate):
 deposition of photoactive Bi2O3 thin films.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              503
_journal_page_last               511
_journal_paper_doi               10.1021/ic402499r
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C84 H168 Bi8 N12 O30, 6(C4 H8 O)'
_chemical_formula_sum            'C108 H216 Bi8 N12 O36'
_chemical_formula_weight         3930.77
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 105.4263(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.1210(2)
_cell_length_b                   27.1155(3)
_cell_length_c                   16.8963(3)
_cell_measurement_reflns_used    128817
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.508
_cell_measurement_theta_min      3.513
_cell_volume                     7119.77(17)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
 DENZO-SCALEPACK Z. Otwinowski and W. Minor, " 
 Processing of X-ray Diffraction Data Collected in Oscillation Mode ", 
 Methods in Enzymology, Volume 276: Macromolecular Crystallography, 
 part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press.
;
_computing_molecular_graphics
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_computing_structure_refinement
;
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. H\"ubschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_structure_solution
; 
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , 
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. 
 (1999) J. Appl. Cryst. 32, 115-119
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '618 1.1 degree images with \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  0.1093
_diffrn_reflns_av_sigmaI/netI    0.0969
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            93257
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.20
_diffrn_reflns_theta_min         3.84
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.921
_exptl_absorpt_correction_T_max  0.5041
_exptl_absorpt_correction_T_min  0.2416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3800
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.426
_refine_diff_density_min         -1.711
_refine_diff_density_rms         0.239
_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     784
_refine_ls_number_reflns         19721
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+0.8278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0864
_reflns_number_gt                13013
_reflns_number_total             19721
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402499r_si_001.cif
_cod_data_source_block           h12alj22
_cod_database_code               4337478