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_4323011
_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         'C34 H40 N2 Ni O2 P2 S4, 2(Cl O4)'
_chemical_formula_structural     'C34 H40 N2 Ni O2 P2 S4, (Cl O4)2'
_chemical_formula_sum            'C34 H40 Cl2 N2 Ni O10 P2 S4'
_chemical_formula_weight         956.47
_chemical_melting_point          ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             97-00-12
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                109.79(1)
_cell_angle_beta                 95.67(2)
_cell_angle_gamma                109.19(1)
_cell_formula_units_Z            1
_cell_length_a                   10.564(1)
_cell_length_b                   11.975(2)
_cell_length_c                   9.124(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294
_cell_measurement_theta_max      17.8
_cell_measurement_theta_min      14.0
_cell_volume                     996.6(3)
_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  0.026
_diffrn_reflns_av_sigmaI/netI    0.060
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3717
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.97
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.466
_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   1.576
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     250
_refine_ls_number_reflns         2658
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          .059
_refine_ls_shift/esd_max         .012
_refine_ls_shift/esd_mean        .003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_obs         .067
_reflns_d_resolution_high        .841
_reflns_d_resolution_low         10.391
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              13
_reflns_limit_k_min              -14
_reflns_limit_l_max              10
_reflns_limit_l_min              0
_reflns_number_observed          2658
_reflns_number_total             3508
_reflns_observed_criterion       refl_observed_if_F____>_4__sigma(F___)
_cod_data_source_file            ic9714753_3.cif
_cod_data_source_block           compound_2_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 (17
times).

'_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_1
_cod_database_code               4323011