Dinitrogen-derived (diarylboryl)diazenido Complexes with Differing Coordination to the Thallium Cation
Bouammali, Amal; Coffinet, Anaïs; Vendier, Laure; Simonneau, Antoine; Dalton Transactions  (2022) –; doi:10.1039/D1DT03905A

data_7709065
_publ_section_title
;
 Dinitrogen-derived (diarylboryl)diazenido Complexes with Differing
 Coordination to the Thallium Cation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03905A
_journal_year                    2022
_chemical_formula_moiety         'C32 H12 B F24, C38 H70 B Cl N2 P4 Tl W'
_chemical_formula_sum            'C70 H82 B2 Cl F24 N2 P4 Tl W'
_chemical_formula_weight         1976.58
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2021-10-07 deposited with the CCDC.	2021-12-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.853(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.49380(4)
_cell_length_b                   20.55530(5)
_cell_length_c                   19.92960(4)
_cell_measurement_reflns_used    9384
_cell_measurement_temperature    110
_cell_measurement_theta_max      26.29
_cell_measurement_theta_min      2.18
_cell_volume                     7642.83(12)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.088
_diffrn_reflns_av_unetI/netI     0.121
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            214287
_diffrn_reflns_theta_full        30.570
_diffrn_reflns_theta_max         30.570
_diffrn_reflns_theta_min         1.456
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.829
_exptl_absorpt_correction_T_max  0.63
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3896
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_refine_diff_density_max         6.89
_refine_diff_density_min         -6.22
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9891
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     940
_refine_ls_number_reflns         14999
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0496
_refine_ls_shift/su_max          0.0015236
_refine_ls_shift/su_mean         0.0000320
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ +*****P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1176
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1173
_reflns_limit_h_max              26
_reflns_limit_h_min              -27
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                12474
_reflns_number_total             23419
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.74
_oxford_diffrn_Wilson_scale      413.27
_oxford_refine_ls_scale          0.038107(3)
_cod_data_source_file            d1dt03905a2.cif
_cod_data_source_block           Amal111220
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        7642.85(14)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C70 H82 B2 Cl1 F24 N2 P4 Tl1 W1'
_cod_database_code               7709065
_oxford_refine_reflns_threshold_expression I>-3.0\s(I)
_refine_ls_r_factor_ref          0.0611
_reflns_number_all               15010