Mononuclear Amido and Binuclear Imido Zirconium Complexes Supported by Dibenzotetraaza[14]annulene Ligands. X-ray Structure of [(Me4taa)Zr(μ-NR)2Zr(NHR)2] (R = Butor 2,6-C6H3Me2)
Georgii I. Nikonov; Alexander J. Blake; Philip Mountford; Inorganic Chemistry 36 (1997) 1107–1112; doi:10.1021/ic961209+

data_4327701
_publ_contact_author
;
 Dr P Mountford
 Department of Chemistry
 University of Nottingham
 Nottingham
 NG7 2RD
;
_publ_contact_author_email       Philip.Mountford@nott.ac.uk
_publ_contact_author_fax         '+44 115 951 3563'
_publ_contact_author_phone       '+44 115 951 3513'
_publ_section_title
;
 Mononuclear Amido and Binuclear Imido Zirconium Complexes Supported by
 Dibenzotetraaza[14]annulene Ligands. X-ray Structure of
 [(Me4taa)Zr(\m-NR)2Zr(NHR)2] (R = Butor 2,6-C6H3Me2)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1107
_journal_page_last               1112
_journal_paper_doi               10.1021/ic961209+
_journal_volume                  36
_journal_year                    1997
_chemical_compound_source
;
 Reaction of Me4taaH2 with [Zr2(mu-N-2,6-C6H3Me2)2(NH-2,6-C6H3Me2)4(py)2]
;
_chemical_formula_moiety         ' C54 H60 N8 Zr2 , (C7 H8)'
_chemical_formula_sum            'C61 H68 N8 Zr2'
_chemical_formula_weight         1095.7
_chemical_name_systematic
;
 [(Me4taa)Zr(mu-N-2,6-C6H3Me2)2Zr(NH-2,6-C6H3Me2)2] . (C7H8)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     SIR92
_audit_creation_date             96-08-14
_audit_creation_method           CRYSTALS
_cell_angle_alpha                90.0
_cell_angle_beta                 123.75(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4.00
_cell_length_a                   25.353(11)
_cell_length_b                   15.394(4)
_cell_length_c                   16.423(4)
_cell_measurement_reflns_used    49
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      16.0
_cell_measurement_theta_min      14.5
_cell_volume                     5329(3)
_computing_cell_refinement       'STADI4 (Stoe & Cie 1995a)'
_computing_data_collection       'STADI4 (Stoe & Cie 1995a)'
_computing_data_reduction
;
X-RED (Stoe & Cie, 1995b)
CRYSTALS (Watkin et al, 1996)
;
_computing_molecular_graphics    'CAMERON (Watkin, Prout and Pearce, 1996)'
_computing_publication_material  'CRYSTALS (Watkin et al, 1996)'
_computing_structure_refinement  'CRYSTALS (Watkin et al, 1996)'
_computing_structure_solution    'SIR92 (Altomare, et al, 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_measurement_device       'STOE STADI4 4-circle-diffractometer D092'
_diffrn_measurement_method       \w-\q
_diffrn_radiation_collimation    '0.8 mm'
_diffrn_radiation_detector       'NaI(Tl) scintillation counter'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  90.0
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_av_sigmaI/netI    0.05688
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6019
_diffrn_reflns_theta_max         25.47
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        7.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.44
_exptl_absorpt_correction_T_max  0.9297
_exptl_absorpt_correction_T_min  0.8340
_exptl_absorpt_correction_type   'psi scans'
_exptl_absorpt_process_details
;
 Mu * R used = 0.05   
 Psi Scan Reflexions used:
    0   0   4 
    4   0   4 
   -2   0   8 
    4   0   4 
   -2   0   8 
    3   1   7 
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       block
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.525
_exptl_crystal_size_min          0.450
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.78
_refine_ls_abs_structure_details 'not determined'
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_coef       'not required'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   3.3226
_refine_ls_hydrogen_treatment    'Riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         3515
_refine_ls_number_restraints     10
_refine_ls_R_factor_obs          0.0425
_refine_ls_shift/esd_max         0.003713
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         0.0475
_reflns_limit_h_max              25
_reflns_limit_h_min              -30
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_observed          3515
_reflns_number_total             4339
_reflns_observed_criterion       >2.00\s(I)
_cod_data_source_file            ic9612092B_2.cif
_cod_data_source_block           COMPOUND8_toluene_adduct
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'unit weights' was changed to
'unit'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'Geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        5332
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        ' C61 H68 N8 Zr2 '
_cod_database_code               4327701