Novel dinuclear dimethylamido-3,5-dimethylpyrazolato and tetranuclear dimethylamido-3,5-dimethylpyrazolato-polyoxo zirconium(iv) complexes. Synthesis and structural characterisation
Sanz, Martial; Mosquera, Marta E. G.; Cuenca, Tomás; Dalton Transactions  (2009) 2616–2622; doi:10.1039/b817574h

data_7000920
_publ_section_title
;
 Novel dinuclear dimethylamido-3,5-dimethylpyrazolato and tetranuclear
 dimethylamido-3,5-dimethylpyrazolato-polyoxo zirconium(iv) complexes.
 Synthesis and structural characterisation
;
_journal_issue                   14
_journal_name_full               'Dalton Transactions'
_journal_page_first              2616
_journal_page_last               2622
_journal_paper_doi               10.1039/b817574h
_journal_year                    2009
_chemical_formula_sum            'C55 H88 N20 O2 Zr4'
_chemical_formula_weight         1426.33
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.67(2)
_cell_angle_beta                 81.670(10)
_cell_angle_gamma                80.161(11)
_cell_formula_units_Z            1
_cell_length_a                   10.2517(9)
_cell_length_b                   12.213(2)
_cell_length_c                   14.484(3)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21.202
_cell_measurement_theta_min      3.25
_cell_volume                     1750.3(5)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_sigmaI/netI    0.0700
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            32949
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.19
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             734
_exptl_crystal_size_max          0.411
_exptl_crystal_size_mid          0.277
_exptl_crystal_size_min          0.164
_platon_squeeze_details
;A molecule of toluene crystallized with every molecule of this compound but
presented severe disorder and it was not possible to get a chemical sensible
model for it, so Squeeze procedure was used to remove their contribution
to the structure factors.
;
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         7987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1167
_reflns_number_gt                5698
_reflns_number_total             7987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b817574h.txt
_cod_data_source_block           4
_cod_database_code               7000920