Synthesis of new structurally constrained tetraaza macropolycyclic compounds containing two rigid bridges: Crystal structure and chemical properties of a copper(II) complex
Shin-Geol Kang; Yun-Taek Lee; Hyungphil Chun; Kimoon Kim; Inorganica Chimica Acta  (2014) 315–319; doi:10.1016/j.ica.2013.09.018

data_1543610
_publ_section_title
;
 Synthesis of new structurally constrained tetraaza macropolycyclic
 compounds containing two rigid bridges: Crystal structure and chemical
 properties of a copper(II) complex
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              315
_journal_page_last               319
_journal_paper_doi               10.1016/j.ica.2013.09.018
_journal_volume                  409B
_journal_year                    2014
_chemical_formula_sum            'C36 H52 Cl2 Cu N4 O8'
_chemical_formula_weight         803.26
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1090(3)
_cell_length_b                   15.7941(2)
_cell_length_c                   13.2947(2)
_cell_measurement_temperature    238(2)
_cell_volume                     3592.51(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      238(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0838
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16977
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_T_max  0.8552
_exptl_absorpt_correction_T_min  0.7765
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             1692
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.54(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         6164
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0394P)^2^+5.1253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1252
_reflns_number_gt                5166
_reflns_number_total             6164
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2014-409B-315-319.cif
_cod_data_source_block           ref
_cod_depositor_comments
;
The following automatic conversions were performed:

'_journal_paper_doi' value 'doi:10.1016/j.ica.2013.09.018' was
changed to '10.1016/j.ica.2013.09.018'.

Automatic conversion script
Id: cif_fix_values 6433 2018-09-21 13:16:33Z andrius 
;
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               1543610