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_4319471
_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     C46H92N30Cu4F24O4P4
_chemical_formula_sum            'C23 H46 Cu2 F12 N15 O2 P2'
_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                91.846(11)
_cell_angle_beta                 98.218(12)
_cell_angle_gamma                105.617(17)
_cell_formula_units_Z            2
_cell_length_a                   12.060(2)
_cell_length_b                   12.554(2)
_cell_length_c                   14.0509(15)
_cell_measurement_temperature    293
_cell_volume                     2022.2(5)
_computing_data_reduction        xtal_DIFDAT_SORTRF_ADDREF_ABSORB
_computing_molecular_graphics    xtal
_computing_publication_material  xtal_BONDLA_CIFIO
_computing_structure_refinement  xtal_CRYLSQ
_computing_structure_solution    xtal
_diffrn_ambient_temperature      296
_diffrn_measurement_device       CAD4
_diffrn_radiation_source         MoKa
_diffrn_radiation_type           xray_tube
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  .036
_diffrn_reflns_av_sigmaI/netI    .092
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7127
_diffrn_reflns_reduction_process perpendicular_monochr_Lp
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.47
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.23
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_F_000             862
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.438
_refine_diff_density_min         -2.95
_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   1.579
_refine_ls_goodness_of_fit_obs   2.169
_refine_ls_matrix_type           atomblock
_refine_ls_number_constraints    0
_refine_ls_number_parameters     506
_refine_ls_number_reflns         3129
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .202
_refine_ls_R_factor_obs          .068
_refine_ls_shift/esd_max         .238
_refine_ls_shift/esd_mean        .05
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .078
_refine_ls_wR_factor_obs         .069
_reflns_d_resolution_high        .842
_reflns_d_resolution_low         13.868
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              16
_reflns_limit_l_min              -16
_reflns_number_observed          3129
_reflns_number_total             7110
_reflns_observed_criterion       refl_observed_if_F____>_.000_sigma(F___)
_cod_data_source_file            ic000991h_3.cif
_cod_data_source_block           '[Cu4Ldur(mu2-N3)4](PF6)4.4H2O.6CH3CN'
_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_cell_volume        2022.1(6)
_cod_original_sg_symbol_Hall     -p_1
_cod_original_formula_sum        'C23 H46 N15 Cu2 F12 O2 P2'
_cod_database_code               4319471
_exptl_absorpt_correction_a_min  1.088
_exptl_absorpt_correction_a_max  1.241