Control of metal/ligand stoichiometry and structure in aminopyridinato complexes of zirconium: N-alkyl is better than trimethylsilyl
Morton, Colin; O’Shaughnessy, Paul; Scott, Peter; Chemical Communications  (2000) 2099–; doi:10.1039/b006603f

data_7111095
_publ_section_title
;
 Control of metal/ligand stoichiometry and structure in aminopyridinato
 complexes of zirconium: N-alkyl is better than trimethylsilyl
;
_journal_issue                   21
_journal_name_full               'Chemical Communications'
_journal_page_first              2099
_journal_paper_doi               10.1039/b006603f
_journal_year                    2000
_chemical_formula_sum            'C45 H72 N4 Zr'
_chemical_formula_weight         760.29
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                89.456(4)
_cell_angle_beta                 79.991(5)
_cell_angle_gamma                87.587(4)
_cell_formula_units_Z            2
_cell_length_a                   11.456(2)
_cell_length_b                   13.352(3)
_cell_length_c                   14.019(3)
_cell_measurement_reflns_used    9057
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.94
_cell_measurement_theta_min      2.65
_cell_volume                     2109.8(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.892
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_sigmaI/netI    0.1461
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20512
_diffrn_reflns_theta_full        29.10
_diffrn_reflns_theta_max         29.10
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.295
_exptl_absorpt_correction_T_max  0.9784
_exptl_absorpt_correction_T_min  0.5597
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.41
_refine_diff_density_max         1.554
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         10117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1584
_reflns_number_gt                6025
_reflns_number_total             10117
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b006603fsup1.cif
_cod_data_source_block           cm23
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2109.9(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7111095