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_7702672
_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_analytical     'C28 H36 Cu N1A O1A'
_chemical_formula_structural     'C28 H36 Cu N1A O1A'
_chemical_formula_sum            'C28 H36 A2 Cu N O'
_chemical_formula_weight         496.13
_chemical_name_common            CuSal-N-Cycloheptyl
_chemical_name_systematic
' bis-{(cycloheptyl)[(2-oxo-1H-benzo-1-ylidene)methyl]-aminato}copper(II) (2)'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_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                 96.53(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.543(2)
_cell_length_b                   10.067(2)
_cell_length_c                   12.624(2)
_cell_measurement_reflns_used    41
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.91
_cell_measurement_theta_min      4.18
_cell_volume                     2467.5(7)
_computing_cell_refinement       'XSCANS V. 4.2 (Siemens 1990)'
_computing_data_collection       'XSCANS V. 4.2 (Siemens 1990)'
_computing_data_reduction        'XSCANS V. 4.2 (Siemens 1990)'
_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, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0716
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5320
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        <3
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_T_max  0.8182
_exptl_absorpt_correction_T_min  0.7777
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1052
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0012(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.874
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0936
_refine_ls_wR_factor_gt          0.0846
_reflns_number_observed          2811
_reflns_number_total             4330
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104892a.txt
_cod_data_source_block           cusalchp
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' 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^)+(0.0381P)^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^)+(0.0381P)^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        2467.5(5)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C28 H36 Cu N1A O1A'
_cod_database_code               7702672
_solved_by                       'Simon Hernandez-Ortega'