NMR Studies of Mononuclear Octahedral Ni(II) Complexes Supported by Tris((2-pyridyl)methyl)amine-Type Ligands
Ewa Szajna; Piotr Dobrowolski; Amy L. Fuller; Atta M. Arif; Lisa M. Berreau; Inorganic Chemistry 43 (2004) 3988–3997; doi:10.1021/ic040002a

data_4311156
_publ_section_title
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 NMR Studies of Mononuclear Octahedral Ni(II) Complexes Supported by
 Tris((2-pyridyl)methyl)amine-Type Ligands
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3988
_journal_page_last               3997
_journal_paper_doi               10.1021/ic040002a
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C36 H35 Cl2 N7 Ni O4'
_chemical_formula_weight         759.32
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.4683(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4913(4)
_cell_length_b                   10.0769(3)
_cell_length_c                   23.3121(5)
_cell_measurement_reflns_used    7357
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_volume                     3589.54(16)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'WinGX, Ortep3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius kappaCCD Diffractometer'
_diffrn_measurement_method       'Phi plus Omega scan'
_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  0.0415
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_diffrn_reflns_limit_h_max       20
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_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            13801
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    0.739
_exptl_absorpt_correction_T_max  0.9365
_exptl_absorpt_correction_T_min  0.7926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
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_refine_ls_extinction_coef       0.0027(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         8095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0743P)^2^+2.6950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.1534
_reflns_number_gt                5603
_reflns_number_total             8095
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic040002a.cif
_cod_data_source_block           usu096
_cod_depositor_comments
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The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_database_code               4311156