Syntheses, Crystal Structures, Magnetic Properties, and EPR Spectra of Tetranuclear Copper(II) Complexes Featuring Pairs of "Roof-Shaped" Cu2X2 Dimers with Hydroxide, Methoxide, and Azide Bridges
Bim Graham; Milton T. W. Hearn; Peter C. Junk; Christopher M. Kepert; Frank E. Mabbs; Boujemaa Moubaraki; Keith S. Murray; Leone Spiccia; Inorganic Chemistry 40 (2001) 1536–1543; doi:10.1021/ic000991h

data_4319469
_publ_section_title
;
 Syntheses, Crystal Structures, Magnetic Properties, and EPR Spectra of
 Tetranuclear Copper(II) Complexes Featuring Pairs of "Roof-Shaped" Cu2X2
 Dimers with Hydroxide, Methoxide, and Azide Bridges
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1536
_journal_page_last               1543
_journal_paper_doi               10.1021/ic000991h
_journal_volume                  40
_journal_year                    2001
_chemical_formula_structural     C34H70N12Cl4O20Cu4
_chemical_formula_sum            'C17 H35 Cl2 Cu2 N6 O10'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             98-08-21
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_cell_angle_alpha                82.228(15)
_cell_angle_beta                 80.794(11)
_cell_angle_gamma                65.715(14)
_cell_formula_units_Z            2
_cell_length_a                   10.2479(12)
_cell_length_b                   12.130(2)
_cell_length_c                   14.353(3)
_cell_measurement_temperature    293
_cell_volume                     1600.6(5)
_computing_data_reduction        xtal
_computing_molecular_graphics    xtal
_computing_publication_material  xtal_CIFIO
_computing_structure_refinement  xtal_CRYLSQ
_computing_structure_solution    xtal
_diffrn_ambient_temperature      293
_diffrn_measurement_device       CAD4
_diffrn_radiation_source         MoKa
_diffrn_radiation_type           xray_tube
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  .018
_diffrn_reflns_av_sigmaI/netI    .051
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5981
_diffrn_reflns_reduction_process perpendicular_monochr_Lp
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.44
_diffrn_standards_decay_%        'approx 50%'
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.55
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_F_000             702
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.40
_refine_diff_density_max         3.487
_refine_diff_density_min         -4.244
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   0
_refine_ls_extinction_coef       .00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   8.04
_refine_ls_goodness_of_fit_obs   10.843
_refine_ls_matrix_type           atomblock
_refine_ls_number_constraints    0
_refine_ls_number_parameters     380
_refine_ls_number_reflns         2600
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .238
_refine_ls_R_factor_obs          .078
_refine_ls_shift/esd_max         1.776
_refine_ls_shift/esd_mean        .425
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .228
_refine_ls_wR_factor_obs         .074
_reflns_d_resolution_high        .842
_reflns_d_resolution_low         14.126
_reflns_limit_h_max              12
_reflns_limit_h_min              0
_reflns_limit_k_max              14
_reflns_limit_k_min              -12
_reflns_limit_l_max              17
_reflns_limit_l_min              -16
_reflns_number_observed          3237
_reflns_number_total             5633
_reflns_observed_criterion       refl_observed_if_F____>_.000_sigma(F___)
_cod_data_source_file            ic000991h_1.cif
_cod_data_source_block           '[Cu4Ldur(mu2-OH)4](ClO4)4'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' 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 
;
_cod_original_sg_symbol_Hall     -p_1
_cod_original_formula_sum        'C17 H35 N6 Cl2 O10 Cu2'
_cod_database_code               4319469
_exptl_absorpt_correction_a_min  1.666
_exptl_absorpt_correction_a_max  2.283