A new C-anionic tripodal ligand 2-{bis(benzothiazolyl)(methoxy)methyl}phenyl and its bismuth complexes.
Shimada, Shigeru; Yin, Shuang-Feng; Bao, Ming; Dalton transactions (Cambridge, England : 2003) 50 (2021) 7949–7954; doi:10.1039/d1dt01071a

data_7707420
_publ_section_title
;
 A new C-anionic tripodal ligand
 2-{bis(benzothiazolyl)(methoxy)methyl}phenyl and its bismuth complexes.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7949
_journal_page_last               7954
_journal_paper_doi               10.1039/d1dt01071a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C44 H30 Bi Cl N4 O2 S4'
_chemical_formula_sum            'C44 H30 Bi Cl N4 O2 S4'
_chemical_formula_weight         1019.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-03-26 deposited with the CCDC.	2021-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                110.088(2)
_cell_angle_beta                 104.112(2)
_cell_angle_gamma                107.625(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3209(3)
_cell_length_b                   13.3170(3)
_cell_length_c                   14.6867(3)
_cell_measurement_reflns_used    9470
_cell_measurement_temperature    153
_cell_measurement_theta_max      28.4790
_cell_measurement_theta_min      1.7970
_cell_volume                     1987.42(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      153
_diffrn_detector                 'Bruker APEX area detector'
_diffrn_detector_area_resol_mean 8.366
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.980
_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      2.31 183.92   0.30   14.99    --   28.00  73.62 -25.69  606
  2  \w      2.31 132.67   0.30   14.99    --   28.00  73.62  64.31  435
  3  \w      2.31  71.24   0.30   14.99    --   28.00  73.62 154.31  230
  4  \w      2.31  17.29   0.30   14.99    --   28.00  73.62 -25.69   50
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0391476000
_diffrn_orient_matrix_UB_12      -0.0337869000
_diffrn_orient_matrix_UB_13      -0.0541384000
_diffrn_orient_matrix_UB_21      0.0525440000
_diffrn_orient_matrix_UB_22      0.0100141000
_diffrn_orient_matrix_UB_23      -0.0133664000
_diffrn_orient_matrix_UB_31      0.0020547000
_diffrn_orient_matrix_UB_32      -0.0517786000
_diffrn_orient_matrix_UB_33      0.0022631000
_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  0.0318
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12258
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         1.602
_diffrn_source                   'Bruker TXS fine-focus rotating anode'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.757
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_description       plate
_exptl_crystal_F_000             1004
_exptl_crystal_recrystallization_method 'crystallized from THF-d8.'
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.740
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         8277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0326P)^2^+5.7098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0781
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7782
_reflns_number_total             8277
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01071a2.cif
_cod_data_source_block           L2BiCl
_cod_depositor_comments
'Adding full bibliography for 7707417--7707423.cif.'
_cod_original_cell_volume        1987.42(9)
_cod_database_code               7707420
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C44 H30 Bi1 Cl1 N4 O2 S4'
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.674
_reflns_odcompleteness_completeness 97.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.67
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13),
 C17(H17), C18(H18), C19(H19), C20(H20), C24(H24), C25(H25), C26(H26), C27(H27),
  C32(H32), C33(H33), C34(H34), C35(H35), C39(H39), C40(H40), C41(H41), C42(H42)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              4469
_shelx_hkl_checksum              82220
_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 1.181
_oxdiff_exptl_absorpt_empirical_full_min 0.822