The effect of phenyl substituents on supramolecular assemblies containing directly linked bis-pyridylimine ligands: synthesis and structural characterisation of mononuclear nickel(ii) and dinuclear silver(i) and cobalt(iii) complexes of (2-pyridyl)phenylketazine
Tuna, Floriana; Clarkson, Guy; Alcock, Nathaniel W.; Hannon, Michael J.; Dalton Transactions  (2003) 2149–; doi:10.1039/b211006g

data_7012447
_publ_section_title
;
 The effect of phenyl substituents on supramolecular assemblies
 containing directly linked bis-pyridylimine ligands: synthesis and
 structural characterisation of mononuclear nickel(ii) and dinuclear
 silver(i) and cobalt(iii) complexes of (2-pyridyl)phenylketazine
;
_journal_issue                   11
_journal_name_full               'Dalton Transactions'
_journal_page_first              2149
_journal_paper_doi               10.1039/b211006g
_journal_year                    2003
_chemical_formula_sum            'C53 H50.5 Co2 F18 N8 O8.25 P3'
_chemical_formula_weight         1484.28
_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                80.385(3)
_cell_angle_beta                 82.541(3)
_cell_angle_gamma                73.978(3)
_cell_formula_units_Z            2
_cell_length_a                   12.2068(18)
_cell_length_b                   13.2943(19)
_cell_length_c                   21.456(3)
_cell_measurement_reflns_used    4636
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      3
_cell_volume                     3286.7(8)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Siemens SMART diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_sigmaI/netI    0.1666
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15747
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plathe
_exptl_crystal_F_000             1503
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.0026(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         10201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.1671
_refine_ls_R_factor_gt           0.0763
_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^)+(0.0970P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.2066
_reflns_number_gt                4967
_reflns_number_total             10201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b211006g.txt
_cod_data_source_block           ft13
_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 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C53 H50.50 Co2 F18 N8 O8.25 P3'
_cod_database_code               7012447