Syntheses and structures of a range of metal complexes with the ligand cis,cis-1,3,5-(E,E)-tris(phenylpropenylideneamino)cyclohexane
Greener, Bryan; Foxon, Simon P.; Walton, Paul H.; New Journal of Chemistry 24 (2000) 269–; doi:10.1039/b000441n

data_7051268
_publ_section_title
;
 Syntheses and structures of a range of metal complexes with the ligand
 cis,cis-1,3,5-(E,E)-tris(phenylpropenylideneamino)cyclohexane
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              269
_journal_paper_doi               10.1039/b000441n
_journal_volume                  24
_journal_year                    2000
_chemical_formula_moiety         'C33 H33 Cl N3 Ni 1+, C24 H20 B 1-'
_chemical_formula_sum            'C57 H53 B Cl N3 Ni'
_chemical_formula_weight         884.99
_chemical_melting_point          495.2(3)
_chemical_name_common            '[Ni(Ph-protach)(Cl)]BPh4, (2)'
_chemical_name_systematic
; 
cis,cis-1,3,5-(E,E)-tri(phenyl-propenylideneamino)cyclohexane
nickel(II) chloride tetraphenylborate, (2) 
{tri(phenyl-propenylideneamino)cyclohexane = (Ph-protach)}  
;
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.335(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.579(3)
_cell_length_b                   16.549(3)
_cell_length_c                   19.916(2)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_volume                     4845.1(14)
_computing_cell_refinement       'MSC/AFC (Diffractometer Control)'
_computing_data_collection       'MSC/AFC (Diffractometer Control)'
_computing_data_reduction
'(teXsan, Molecular Structure Corporation, 1992)'
_computing_molecular_graphics    teXsan
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SAPI91 (Rigaku Corporation, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.804
_diffrn_measured_fraction_theta_max 0.804
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7496
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.69
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.344
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.797
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         6868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0969P)^2^+3.7150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1934
_reflns_number_gt                4119
_reflns_number_total             6868
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b000441n.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '495-495.5 K' was changed to
'495.2(3)' - the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        4845.1(13)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7051268