Synthesis, crystal structures, spectroscopic and electrochemical properties of homologous series of copper(II) complexes of Schiff bases derived from cycloalkylamines
Aguilar-Martínez, Martha; Saloma-Aguilar, Ricardo; Macías-Ruvalcaba, Norma; Cetina-Rosado, Raúl; Navarrete-Vázquez, Agustina; Gómez-Vidales, Virginia; Zentella-Dehesa, Arturo; Toscano, Rubén A.; Hernández-Ortega, Simón; Fernández-G., Juan M.; Journal of the Chemical Society, Dalton Transactions  (2001) 2346–; doi:10.1039/b104892a

data_7702676
_publ_section_title
;
 Synthesis, crystal structures, spectroscopic and electrochemical
 properties of homologous series of copper(II) complexes of Schiff bases
 derived from cycloalkylamines
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2346
_journal_paper_doi               10.1039/b104892a
_journal_year                    2001
_chemical_formula_sum            'C76 H88 Cu2 N4 O4'
_chemical_formula_weight         1248.58
_chemical_name_common            Cu-1,2-N-cyclooctyl
_chemical_name_systematic
' bis-{(cyclooctyl)[(2-oxo-1H-naphth-1-ylidene)methyl]-aminato}copper(II) (6)'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                93.26(2)
_cell_angle_beta                 101.15(3)
_cell_angle_gamma                98.57(4)
_cell_formula_units_Z            2
_cell_length_a                   13.739(4)
_cell_length_b                   14.054(3)
_cell_length_c                   17.212(3)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.60
_cell_measurement_theta_min      5.40
_cell_volume                     3211.7(14)
_computing_cell_refinement       'XSCANS Ver. 2.1, (SIEMENS 1994)'
_computing_data_collection       'XSCANS Ver. 2.1, (SIEMENS 1994)'
_computing_data_reduction        'XSCANS Ver. 2.1, (SIEMENS 1994)'
_computing_molecular_graphics    'XP, SHELXTL PC Ver  4.2 (sheldrick, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens P4/PC'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_sigmaI/netI    0.1236
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11829
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        <5
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  0.8695
_exptl_absorpt_correction_T_min  0.7619
_exptl_absorpt_correction_type
'semi-empirical based on psi-scan data collection'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       'no applied'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.796
_refine_ls_hydrogen_treatment    'no refined'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         11313
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      0.804
_refine_ls_R_factor_all          0.1381
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.868
_refine_ls_shift/su_mean         0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1446
_reflns_number_gt                4876
_reflns_number_total             11313
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104892a.txt
_cod_data_source_block           cu12ncy-octyl
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        3211.6(11)
_cod_database_code               7702676
_solved_by                       'Simon Hernandez-Ortega'