Triphenylbismuth(v) di[(iso)nicotinates] - transmetallation agents or divergent organometalloligands? First organobismuth(v)-based silver(i) coordination polymers.
Ben Kiran, Ahmad; Mocanu, Teodora; Pöllnitz, Alpár; Shova, Sergiu; Andruh, Marius; Silvestru, Cristian; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2531–2542; doi:10.1039/c7dt04516f

data_7045298
_publ_section_title
;
 Triphenylbismuth(v) di[(iso)nicotinates] - transmetallation agents or
 divergent organometalloligands? First organobismuth(v)-based silver(i)
 coordination polymers.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2531
_journal_page_last               2542
_journal_paper_doi               10.1039/c7dt04516f
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C31 H25 Ag Bi Cl2 N2 O4, F6 Sb'
_chemical_formula_sum            'C31 H25 Ag Bi Cl2 F6 N2 O4 Sb'
_chemical_formula_weight         1113.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-11-14 deposited with the CCDC.
2018-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                83.744(4)
_cell_angle_beta                 71.929(4)
_cell_angle_gamma                76.436(4)
_cell_formula_units_Z            2
_cell_length_a                   10.5410(6)
_cell_length_b                   10.8892(5)
_cell_length_c                   16.7211(7)
_cell_measurement_reflns_used    4867
_cell_measurement_temperature    199.95(10)
_cell_measurement_theta_max      27.0420
_cell_measurement_theta_min      1.9300
_cell_volume                     1772.37(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      199.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -7.00  21.00   1.00    4.00    --  -15.60 -99.00 120.00   28
  2  \w     65.00  90.00   1.00    4.00    --   17.79-178.00  30.00   25
  3  \w    -29.00  51.00   1.00    4.00    --  -15.60  38.00 150.00   80
  4  \w      5.00  61.00   1.00    4.00    --   17.79  57.00 120.00   56
  5  \w    -42.00  49.00   1.00    4.00    --  -15.60  77.00   0.00   91
  6  \w    -83.00  11.00   1.00    4.00    --  -15.60 -77.00-120.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0569602000
_diffrn_orient_matrix_UB_12      0.0280337000
_diffrn_orient_matrix_UB_13      -0.0066778000
_diffrn_orient_matrix_UB_21      0.0085150000
_diffrn_orient_matrix_UB_22      0.0046564000
_diffrn_orient_matrix_UB_23      -0.0439211000
_diffrn_orient_matrix_UB_31      -0.0439281000
_diffrn_orient_matrix_UB_32      0.0607389000
_diffrn_orient_matrix_UB_33      0.0045170000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0798
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12588
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.925
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.476
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.086
_exptl_crystal_description       prism
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.792
_refine_diff_density_min         -1.443
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         6253
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0356P)^2^+1.9211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5321
_reflns_number_total             6253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04516f2.cif
_cod_data_source_block           shi_3308_maan
_cod_depositor_comments
'Adding full bibliography for 7045295--7045303.cif.'
_cod_original_cell_volume        1772.38(15)
_cod_database_code               7045298
_chemical_oxdiff_formula         'C20 H20 O6 N4 Bi1 Ag1 F6'
_chemical_oxdiff_usercomment     TM_33
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C23) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-09-29
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.623
_oxdiff_exptl_absorpt_empirical_full_min 0.547