Tantalum(iv) pyrazolate: new wine in the old wineskin
Petrov, Pavel A.; Laricheva, Yuliya A.; Sukhikh, Taisiya S.; Sokolov, Maxim N.; New Journal of Chemistry 45 (2021) 7047–7051; doi:10.1039/D1NJ00195G

data_7060458
_publ_section_title
;
 Tantalum(iv) pyrazolate: new wine in the old wineskin
;
_journal_issue                   16
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7047
_journal_page_last               7051
_journal_paper_doi               10.1039/D1NJ00195G
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C24 H24 N16 Ta2'
_chemical_formula_sum            'C24 H24 N16 Ta2'
_chemical_formula_weight         898.49
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-11-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-04 deposited with the CCDC.	2021-03-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.76(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4335(17)
_cell_length_b                   14.985(3)
_cell_length_c                   22.574(5)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      35.11
_cell_measurement_theta_min      2.79
_cell_volume                     2833.0(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'Bruker APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            22936
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.697
_diffrn_reflns_theta_min         2.269
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    7.766
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.5198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0922 before and 0.0494 after correction. The Ratio of minimum to maximum transmission is 0.6959. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.107
_exptl_crystal_description       prism
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.700
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         7278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0232
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+6.5592P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0525
_refine_ls_wR_factor_ref         0.0542
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6525
_reflns_number_total             7278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj00195g2.cif
_cod_data_source_block           2
_cod_depositor_comments          'Adding full bibliography for 7060458.cif.'
_cod_database_code               7060458
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.511
_shelx_estimated_absorpt_t_min   0.306
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C23(H23), C24(H24), C25(H25), C33(H33),
 C34(H34), C35(H35), C43(H43), C44(H44), C45(H45), C53(H53), C54(H54), C55(H55),
  C63(H63), C64(H64), C65(H65), C73(H73), C74(H74), C75(H75), C83(H83),
 C84(H84), C85(H85)
;
_shelx_res_checksum              99566
_olex2_submission_special_instructions 'No special instructions were received'