Synthesis, Crystal Structure, and Magnetic Properties of an Alkoxo-Hydroxo-Bridged Octanuclear Copper(II) Complex Showing Chemically Significant Hydrogen-Bonding Interactions Involving a Metallamacrocyclic Core
Arindam Mukherjee; Indranil Rudra; Munirathinam Nethaji; Suryanarayanasastry Ramasesha; Akhil R. Chakravarty; Inorganic Chemistry 42 (2003) 463–468; doi:10.1021/ic020399n

data_4312916
_publ_section_title
;
 Synthesis, Crystal Structure, and Magnetic Properties of an
 Alkoxo-Hydroxo-Bridged Octanuclear Copper(II) Complex Showing Chemically
 Significant Hydrogen-Bonding Interactions Involving a Metallamacrocyclic
 Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              463
_journal_page_last               468
_journal_paper_doi               10.1021/ic020399n
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C68 H64 Cu8 N8 O16'
_chemical_formula_weight         1757.59
_chemical_name_systematic
;
  ?
;
_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                 125.33(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.365(3)
_cell_length_b                   14.320(2)
_cell_length_c                   19.019(2)
_cell_measurement_temperature    293(2)
_cell_volume                     6747(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 for windows (Farrugia, 1997)'
_computing_publication_material  'WINGX publication routines (Farrugia, 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 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker SMART CCD 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  0.1135
_diffrn_reflns_av_sigmaI/netI    0.1162
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20282
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    2.546
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Hexagonal
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.149
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.872
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0536P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1311
_reflns_number_gt                4589
_reflns_number_total             7864
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020399n.cif
_cod_data_source_block           ic020399n
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        6746.7(13)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4312916
_exptl_absorpt_correction_t_min_t_max_ratio 0.828