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_7051269
_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 Zn 1+, C24 H20 B 1-, 3(C H2 Cl2)'
_chemical_formula_sum            'C60 H59 B Cl7 N3 Zn'
_chemical_formula_weight         1146.43
_chemical_melting_point          509.5(5)
_chemical_name_common            '[Zn(Ph-protach)(Cl)]BPh4, (3)'
_chemical_name_systematic
; 
cis,cis-1,3,5-(E,E)-tri(phenyl-propenylideneamino)cyclohexane zinc(II)
chloride tetraphenylborate, (3)
{tri(phenyl-propenylideneamino)cyclohexane = (Ph-protach)}
;
_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                99.61(6)
_cell_angle_beta                 103.87(7)
_cell_angle_gamma                76.73(4)
_cell_formula_units_Z            2
_cell_length_a                   15.222(10)
_cell_length_b                   19.097(9)
_cell_length_c                   10.784(10)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_volume                     2941(4)
_computing_cell_refinement       'AFC/MSC (Diffractometer Control)'
_computing_data_collection       'AFC/MSC (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 0.864
_diffrn_measured_fraction_theta_max 0.864
_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    0.0725
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9459
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.64
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.186
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.775
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         9028
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1414
_refine_ls_R_factor_gt           0.0733
_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^)+(0.1117P)^2^+5.0561P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1853
_refine_ls_wR_factor_ref         0.2276
_reflns_number_gt                5460
_reflns_number_total             9028
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b000441n.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '509-510' was changed to '509.5(5)' -
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_database_code               7051269