Coordination variety of phenyltetrazolato and dimethylamido ligands in dimeric Ti, Zr, and Ta complexes.
Bikzhanova, Galina A.; Guzei, Ilia A.; Acta crystallographica. Section C, Structural chemistry 80 (2024) –; doi:10.1107/S2053229624007411

data_2312590
_publ_section_title
;
 Coordination variety of phenyltetrazolato and dimethylamido ligands in
 dimeric Ti, Zr, and Ta complexes.
;
_journal_coeditor_code           EF3059
_journal_issue                   9
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi               10.1107/S2053229624007411
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac
'[Zr2 (C7 H5 N4)6 (C2 H6 N)2 (C2 H7 N)2], 1.118C6 H6, 0.382C H2 Cl2'
_chemical_formula_moiety
'C50 H56 N28 Zr2, 0.382(C H2 Cl2), 1.118(C6 H6)'
_chemical_formula_sum            'C57.09 H63.47 Cl0.76 N28 Zr2'
_chemical_formula_weight         1351.41
_chemical_name_systematic
;Bis(dimethylamido)-1\k<i>N</i>,2\k<i>N</i>-bis(dimethylamine)-1\k<i>N</i>,2\k<i>N</i>-tris(\m-5-phenyltetrazolato-1:2\k^2^<i>N</i>^2^:<i>N</i>^3^)tris(5-phenyltetrazolato)-1\k^2^<i>N</i>^2^;2\k^2^<i>N</i>^2^,<i>N</i>^3^-
dizirconium(III)]--benzene--dichloromethane (1/1.12/0.38)
;
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2024.06.15 svn.r5e56dd67 for OlexSys, GUI svn.r6981)
;
_cell_angle_alpha                86.9020(10)
_cell_angle_beta                 81.1540(10)
_cell_angle_gamma                89.9690(10)
_cell_formula_units_Z            4
_cell_length_a                   13.9631(5)
_cell_length_b                   16.7619(6)
_cell_length_c                   27.3054(9)
_cell_measurement_reflns_used    7364
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.390
_cell_measurement_theta_min      2.255
_cell_volume                     6305.3(4)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
APEX3 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2008)
;
_computing_structure_solution
;
olex2.solve (Bourhis <i>et al.</i>,  2015)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            70012
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.402
_diffrn_reflns_theta_min         1.551
_diffrn_source_current           40.0
_diffrn_source_power             1.6
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2018)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       block
_exptl_crystal_F_000             2780
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.983
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1671
_refine_ls_number_reflns         25682
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0515P)^2^+3.6611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                20488
_reflns_number_total             25682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ef3059.cif
_cod_data_source_block           2
_cod_database_code               2312590
_shelx_estimated_absorpt_t_min   0.848
_shelx_estimated_absorpt_t_max   0.920
_shelx_hkl_checksum              55350
_shelx_res_checksum              81132