Synthesis and Reactivity of Nickel(II) Complexes of the Pyridine-Based Phosphorus-Containing Macrocycle 6-Phenyl-15-aza-6-phospha-3,9- dithiabicyclo[9,3,1]pentadeca-1(15),11,13-triene
Lluis Escriche; José Antonio Muñoz; Joan Rosell; Raikko Kivekäs; Reijo Sillanpää; Jaume Casabó; Inorganic Chemistry 37 (1998) 4807–4813; doi:10.1021/ic9714753

data_4323010
_publ_contact_author
;    Prof. Lluis Escriche
     Departament de Qu\`imica
     Universitat Aut\'onoma de Barcelona
     08193 Bellaterra
     Barcelona
     Spain
;
_publ_contact_author_email       iqicasabo@cc.uab.es
_publ_contact_author_fax         '34 3 5813101'
_publ_contact_author_phone       '34 3 5811606'
_publ_section_title
;
 Synthesis and Reactivity of Nickel(II) Complexes of the Pyridine-Based
 Phosphorus-Containing Macrocycle 6-Phenyl-15-aza-6-phospha-3,9-
 dithiabicyclo[9,3,1]pentadeca-1(15),11,13-triene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4807
_journal_page_last               4813
_journal_paper_doi               10.1021/ic9714753
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C21 H26 N3 Ni P S2, 2(Cl O4)'
_chemical_formula_structural     'C21 H26 N3 Ni P S2, (Cl O4)2'
_chemical_formula_sum            'C21 H26 Cl2 N3 Ni O8 P S2'
_chemical_formula_weight         673.15
_chemical_melting_point          ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             97-00-12
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                90.00000
_cell_angle_beta                 107.554(8)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   12.704(2)
_cell_length_b                   13.538(2)
_cell_length_c                   17.377(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      16.8
_cell_measurement_theta_min      12.5
_cell_volume                     2849.4(7)
_computing_cell_refinement
;
MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 
1993)
;
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 
1993)
;
_computing_data_reduction
;
Texsan Process (Molecular Structure Corporation ,1993)
;
_computing_molecular_graphics    xtal_ORTEP
_computing_publication_material  xtal_BONDLA_CIFIO
_computing_structure_refinement  'xtal_CRYLSQ (Hall, Flack & Stewart, 1992)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      294
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_av_sigmaI/netI    0.072
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5503
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.12
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1383.79
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         .831
_refine_diff_density_min         -.726
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_coef       .00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   2.242
_refine_ls_hydrogen_treatment    geom
_refine_ls_matrix_type           atomblock
_refine_ls_number_constraints    0
_refine_ls_number_parameters     334
_refine_ls_number_reflns         3083
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.071
_refine_ls_shift/esd_max         .026
_refine_ls_shift/esd_mean        .002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         .076
_reflns_d_resolution_high        .841
_reflns_d_resolution_low         9.027
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_observed          3087
_reflns_number_total             5251
_reflns_observed_criterion       refl_observed_if_F____>_4__sigma(F___)
_cod_data_source_file            ic9714753_2.cif
_cod_data_source_block           compound_1_for_IC9714753
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_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 (21
time).

'_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 (20 times).

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z 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_sg_symbol_Hall     -P_2ybc
_cod_database_code               4323010