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_7051267
_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 Cu N3 2+, O4 S 2-, C1.5 H6 O1.5'
_chemical_formula_sum            'C34.5 H39 Cu N3 O5.5 S'
_chemical_formula_weight         679.29
_chemical_melting_point          549.2(3)
_chemical_name_common            '[Cu(Ph-protach)(SO4)(0.5CH3OH)], (1)'
_chemical_name_systematic
; 
cis,cis-1,3,5-(E,E)-tri(phenyl-propenylideneamino)cyclohexane 
copper sulfate, (1) 
{tri(phenyl-propenylideneamino)cyclohexane = (Ph-protach)} 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 109.49(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.056(5)
_cell_length_b                   17.494(3)
_cell_length_c                   14.397(4)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_volume                     3337.3(17)
_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  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SAPI91 (Rigaku Corporation, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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    0.0490
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6114
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.74
_diffrn_source_current           30
_diffrn_source_voltage           50
_diffrn_standards_decay_%        0.045
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  0.6573
_exptl_absorpt_correction_T_min  0.6170
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.6
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         5644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0646P)^2^+3.4458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1487
_reflns_number_gt                3642
_reflns_number_total             5644
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b000441n.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '549-549.5 K' was changed to
'549.2(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        3337.3(15)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C34.50 H39 Cu N3 O5.5 S'
_cod_database_code               7051267