Isolation, structural and spectroscopic investigations of complexes with tridentate [O,P,O] and [O,O,O] donor ligands
Siefert, Rolf; Weyhermüller, Thomas; Chaudhuri, Phalguni; Journal of the Chemical Society, Dalton Transactions  (2000) 4656–; doi:10.1039/b005693f

data_7010078
_publ_section_title
;
 Isolation, structural and spectroscopic investigations of complexes
 with tridentate [O,P,O] and [O,O,O] donor ligands
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4656
_journal_paper_doi               10.1039/b005693f
_journal_year                    2000
_chemical_formula_sum            'C68 H92 Ni O4 P2'
_chemical_formula_weight         1094.07
_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
_cell_angle_alpha                89.99(2)
_cell_angle_beta                 79.00(2)
_cell_angle_gamma                72.07(2)
_cell_formula_units_Z            2
_cell_length_a                   13.432(1)
_cell_length_b                   15.174(2)
_cell_length_c                   17.048(2)
_cell_measurement_reflns_used    5394
_cell_measurement_temperature    100(2)
_cell_volume                     3238.8(8)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SAINT'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens ShelXTL'
_computing_publication_material  'Siemens ShelXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Siemens SMART CCD-Detector'
_diffrn_measurement_method       '\w-scan, 0.3 deg./frame'
_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  0.1033
_diffrn_reflns_av_sigmaI/netI    0.1202
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24941
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.393
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   'Gaussian Face-Indexed'
_exptl_crystal_colour            'yellow greenish'
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_description       'Transparent Plate '
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.979
_refine_ls_goodness_of_fit_obs   1.070
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         10960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_obs          0.0589
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1412
_refine_ls_wR_factor_obs         0.1193
_reflns_number_observed          6917
_reflns_number_total             11020
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b005693f.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0629P)^2^+0.0000P] 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^)+(0.0629P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3238.8(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7010078