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_7707417
_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         'C22 H15 Br N2 O S2'
_chemical_formula_sum            'C22 H15 Br N2 O S2'
_chemical_formula_weight         467.39
_chemical_name_systematic
2,2'-((2-bromophenyl)(methoxy)methylene)bis(benzo[d]thiazole)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_audit_update_record
;
2021-03-26 deposited with the CCDC.	2021-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   29.9380(7)
_cell_length_b                   18.6991(4)
_cell_length_c                   13.9399(3)
_cell_measurement_reflns_used    10897
_cell_measurement_temperature    153
_cell_measurement_theta_max      28.7360
_cell_measurement_theta_min      1.8600
_cell_volume                     7803.7(3)
_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 1.000
_diffrn_measured_fraction_theta_max 0.985
_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 2.30 183.91 0.30 9.99 -- 28.00 73.65 -25.70 606
 2 \w 2.30 132.66 0.30 9.99 -- 28.00 73.65 64.30 435
 3 \w 2.30 71.23 0.30 9.99 -- 28.00 73.65 154.30 230
 4 \w 2.30 17.28 0.30 9.99 -- 28.00 73.65 -25.70 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      -0.0188993000
_diffrn_orient_matrix_UB_12      0.0113824000
_diffrn_orient_matrix_UB_13      0.0266269000
_diffrn_orient_matrix_UB_21      -0.0127099000
_diffrn_orient_matrix_UB_22      -0.0284170000
_diffrn_orient_matrix_UB_23      -0.0197668000
_diffrn_orient_matrix_UB_31      0.0065279000
_diffrn_orient_matrix_UB_32      -0.0224045000
_diffrn_orient_matrix_UB_33      0.0385964000
_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  0.0176
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11834
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.866
_diffrn_reflns_theta_min         1.945
_diffrn_source                   'Bruker TXS fine-focus rotating anode'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.337
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90919
_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    1.591
_exptl_crystal_description       prism
_exptl_crystal_F_000             3776
_exptl_crystal_recrystallization_method 'crystallized from benzene'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 1778 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4352
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0626P)^2^+29.5270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.822
_reflns_Friedel_fraction_full    0.930
_reflns_Friedel_fraction_max     0.879
_reflns_number_gt                4177
_reflns_number_total             4352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01071a2.cif
_cod_data_source_block           Ligand-precursor
_cod_depositor_comments
'Adding full bibliography for 7707417--7707423.cif.'
_cod_database_code               7707417
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C22 H15 Br N2 O S2'
_reflns_odcompleteness_completeness 98.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_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)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
;
_shelx_res_checksum              21416
_shelx_hkl_checksum              93654
_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 1.084
_oxdiff_exptl_absorpt_empirical_full_min 0.892