Late-Transition-Metal Complexes of BINOL-Derived Salens: Synthesis, Structure, and Reactivity
DiMauro, Erin F.; Kozlowski, Marisa C.; Organometallics 21 (2002) 1454–; doi:10.1021/om010571f

data_4076631
_publ_section_title
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 Late-Transition-Metal Complexes of BINOL-Derived Salens:&#x00A0;
 Synthesis, Structure, and Reactivity
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1454
_journal_paper_doi               10.1021/om010571f
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C49 H38 Cl6 N2 Ni O4'
_chemical_formula_weight         990.22
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.040(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9158(5)
_cell_length_b                   17.2044(8)
_cell_length_c                   18.3523(6)
_cell_measurement_temperature    200(2)
_cell_volume                     4674.0(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_measurement_device       'image plate area detector'
_diffrn_measurement_device_type  'Rigaku R-AXIS IIc'
_diffrn_measurement_method       'phi oscillations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_sigmaI/netI    0.0704
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19661
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    0.804
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.075
_refine_ls_goodness_of_fit_obs   1.123
_refine_ls_matrix_type           full
_refine_ls_number_parameters     992
_refine_ls_number_reflns         13389
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.075
_refine_ls_restrained_S_obs      1.123
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_obs          0.0948
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1035P)^2^+14.8947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2414
_refine_ls_wR_factor_obs         0.2276
_reflns_number_observed          10993
_reflns_number_total             13389
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om010571f.cif
_cod_data_source_block           koz836
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1035P)^2^+14.8947P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1035P)^2^+14.8947P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21       '
_cod_database_code               4076631