An unusual [4 + 4 + 4] bishelical complex, Cu3(H2L)(L)·2H2O [H4L′ = N,N′-bis(3-hydroxysalicylidene)-1,4-diaminobutane]: synthesis and crystal structure
Sanmartín, Jesús; Bermejo, Manuel R.; García-Deibe, Ana M.; Piro, Oscar; Castellano, Eduardo E.; Chemical Communications  (1999) 1953–; doi:10.1039/a905133c

data_7110639
_publ_section_title
;
 An unusual [4 + 4 + 4] bishelical complex, Cu3(H2L)(L)&#x00B7;2H2O
 [H4L&#x2032; = N,N&#x2032;-bis(3-hydroxysalicylidene)-1,4-diaminobutane]:
 synthesis and crystal structure
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_journal_issue                   19
_journal_name_full               'Chemical Communications'
_journal_page_first              1953
_journal_paper_doi               10.1039/a905133c
_journal_year                    1999
_chemical_formula_moiety         'C36 H38 Cu3 N4 O10'
_chemical_formula_sum            'C36 H38 Cu3 N4 O10'
_chemical_formula_weight         877.32
_chemical_name_common            Cu3(H2L)(L).2H2O
_chemical_name_systematic
;
 ?
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_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 110.0630(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.098(7)
_cell_length_b                   13.871(6)
_cell_length_c                   15.366(7)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.96
_cell_measurement_theta_min      6.39
_cell_volume                     3423(3)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta 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  0.1647
_diffrn_reflns_av_sigmaI/netI    0.3419
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3146
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  30
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.914
_exptl_absorpt_correction_T_max  0.8617
_exptl_absorpt_correction_T_min  0.7864
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
a grid of  8 x  8 x  8 =   512 sampling points was used
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1796
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.915
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3021
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.2971
_refine_ls_R_factor_gt           0.0610
_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^)+(0.0967P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.2272
_reflns_number_gt                872
_reflns_number_total             3021
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            905133csup1.cif
_cod_data_source_block           s93
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        3423(2)
_cod_original_sg_symbol_H-M      'C2/c (No 15)'
_cod_database_code               7110639
_diffrn_standards_decay_corr_max 1.047
_diffrn_standards_decay_corr_min 0.926