A Sterically Hindered N,N,O Tripod Ligand and Its Zinc Complex Chemistry
Alexander Trösch; Heinrich Vahrenkamp; Inorganic Chemistry 40 (2001) 2305–2311; doi:10.1021/ic001204j

data_4319616
_publ_section_title
;
 A Sterically Hindered N,N,O Tripod Ligand and Its Zinc Complex Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2305
_journal_page_last               2311
_journal_paper_doi               10.1021/ic001204j
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C82 H106 Cl N9 O13 Zn3'
_chemical_formula_weight         1657.32
_chemical_melting_point          195
_chemical_name_common            Tris(Di(2-picolyl)(2-hydroxylato-3,5-di-tert-b
_chemical_name_systematic        Tris(Di(2-picolyl)(2-hydroxylato-3,5-di-tert-b
_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                92.16(3)
_cell_angle_beta                 115.67(3)
_cell_angle_gamma                106.65(3)
_cell_formula_units_Z            2
_cell_length_a                   16.888(3)
_cell_length_b                   16.919(3)
_cell_length_c                   19.163(4)
_cell_measurement_temperature    180(2)
_cell_volume                     4644(2)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_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  0.0740
_diffrn_reflns_av_sigmaI/netI    0.1155
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29785
_diffrn_reflns_theta_full        23.58
_diffrn_reflns_theta_max         23.58
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       isometric
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.372
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    'Riding Model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     995
_refine_ls_number_reflns         13386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.718
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1468P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2072
_refine_ls_wR_factor_ref         0.2380
_reflns_number_gt                8021
_reflns_number_total             13386
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001204j_1.cif
_cod_data_source_block           a27(k5)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_angle_publ_flag' value 'Y' changed to 'y' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (225 times).

'_geom_bond_publ_flag' value 'Y'
changed to 'y' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (124
times).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        4644.3(16)
_cod_database_code               4319616