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_7045296
_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         'C62 H46 Ag2 Bi2 F6 N4 O14 S2, 2(C H2 Cl2)'
_chemical_formula_sum            'C64 H50 Ag2 Bi2 Cl4 F6 N4 O14 S2'
_chemical_formula_weight         2052.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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
_audit_creation_date             2016-10-24
_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                90
_cell_angle_beta                 90.574(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3800(4)
_cell_length_b                   19.8689(8)
_cell_length_c                   28.0926(9)
_cell_measurement_reflns_used    6581
_cell_measurement_temperature    130.1(2)
_cell_measurement_theta_max      27.8690
_cell_measurement_theta_min      2.0440
_cell_volume                     6909.8(4)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130.1(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1593
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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    -18.00  12.00   1.00  100.00    --  -15.29 -99.00   0.00   30
  2  \w    -30.00  48.00   1.00  100.00    --  -15.29  19.00   0.00   78
  3  \w     37.00  78.00   1.00  100.00    --   17.55  57.00  30.00   41
  4  \w    -17.00  21.00   1.00  100.00    --  -15.29 -96.00-104.00   38
  5  \w    -87.00 -35.00   1.00  100.00    --  -15.29-178.00  90.00   52
;
_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      -0.0000943000
_diffrn_orient_matrix_UB_12      0.0284895000
_diffrn_orient_matrix_UB_13      0.0152290000
_diffrn_orient_matrix_UB_21      0.0247258000
_diffrn_orient_matrix_UB_22      0.0194482000
_diffrn_orient_matrix_UB_23      -0.0180514000
_diffrn_orient_matrix_UB_31      -0.0516759000
_diffrn_orient_matrix_UB_32      0.0092061000
_diffrn_orient_matrix_UB_33      -0.0089383000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0836
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            29329
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.791
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.934
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67454
_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    1.973
_exptl_crystal_description       prism
_exptl_crystal_F_000             3952
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.277
_refine_diff_density_min         -1.647
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         12047
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0665
_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^)+(0.0414P)^2^+106.0104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1365
_refine_ls_wR_factor_ref         0.1531
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8606
_reflns_number_total             12047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04516f2.cif
_cod_data_source_block           shi_3157_maan
_cod_depositor_comments
'Adding full bibliography for 7045295--7045303.cif.'
_cod_database_code               7045296
_chemical_oxdiff_formula         'C30 H30 N4 O10 S2 F6 Ag1 Bi1'
_chemical_oxdiff_usercomment     TM_17
_reflns_odcompleteness_completeness 98.39
_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. Restrained distances
 S2X-O7X \\sim S1B-O7B \\sim S2X-O5X \\sim S2X-O5B \\sim S1B-O5B \\sim S1B-O6B
 with sigma of 0.01
 O7B-O6B \\sim O7B-O5B \\sim O6B-O5B \\sim O7X-O6X \\sim O7X-O5X \\sim O6X-O5X
 with sigma of 0.01
 F1A-C31A \\sim F2A-C31A \\sim F3A-C31A \\sim F5X-C19 \\sim F3B-C31B \\sim
F1B-C31B \\sim F2B-C31B ~
 F6X-C19 \\sim F4X-C19
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uiso(F5X) = Uiso(C19) = Uiso(F6X) = Uiso(S2X) = Uiso(F4X) = Uiso(O5X) =
Uiso(O7X) = Uiso(O5B) = Uiso(O5B) = Uiso(S1B) = Uiso(O7B) = Uiso(O6B) =
Uiso(C31B) = Uiso(F1B) = Uiso(F2B) = Uiso(F3B)
4. Others
 Sof(S1B)=Sof(F1B)=Sof(O5B)=Sof(O6B)=Sof(O7B)=Sof(C31B)=1-FVAR(1)
 Sof(S2X)=Sof(F4X)=Sof(O5X)=Sof(O6X)=Sof(O7X)=Sof(C19)=FVAR(1)
 Sof(F5X)=Sof(F6X)=1-FVAR(2)
 Sof(F2B)=Sof(F3B)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C32A(H32A,H32B), C32B(H32C,H32D)
5.b Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C3B(H3B), C4A(H4A), C4B(H4B), C5A(H5A), C5B(H5B), C6A(H6A),
 C6B(H6B), C9A(H9A), C9B(H9B), C10A(H10A), C10B(H10B), C11A(H11A), C11B(H11B),
 C12A(H12A), C12B(H12B), C14A(H14A), C14B(H14B), C15A(H15A), C15B(H15B),
 C16A(H16A), C16B(H16B), C17A(H17A), C17B(H17B), C18A(H18A), C18B(H18B),
 C20A(H20A), C20B(H20B), C21A(H21A), C21B(H21B), C22A(H22A), C22B(H22B),
 C23A(H23A), C23B(H23B), C24A(H24A), C24B(H24B), C26A(H26A), C26B(H26B),
 C27A(H27A), C27B(H27B), C28A(H28A), C28B(H28B), C29A(H29A), C29B(H29B),
 C30A(H30A), C30B(H30B)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-04-05
_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 1.539
_oxdiff_exptl_absorpt_empirical_full_min 0.769