New Phenoxido-Bridged Quasi-Tetrahedral and Rhomboidal [Cu4] Compounds Bearing μ4-Oxido or μ1,1-Azido Ligands: Synthesis, Chemical Reactivity, and Magnetic Studies
Mrinal Sarkar; Rodolphe Clérac; Corine Mathonière; Nigel G. R. Hearns; Valerio Bertolasi; Debashis Ray; Inorganic Chemistry 50 (2011) 3922–3933; doi:10.1021/ic102226j

data_4324942
_publ_contact_author_address
; Department of Chemistry 
 Indian Institute of Technology
 Kharagpur-721302
 India
;
_publ_contact_author_email       deposit@ccdc.cam.ac.uk
_publ_contact_author_fax         ' 913222-255303'
_publ_contact_author_name        ' Prof. Debashis Ray'
_publ_contact_author_phone       ' 03222-283324'
_publ_section_title
;
 New Phenoxido-Bridged Quasi-Tetrahedral and Rhomboidal [Cu4] Compounds
 Bearing \m4-Oxido or \m1,1-Azido Ligands: Synthesis, Chemical Reactivity,
 and Magnetic Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3922
_journal_page_last               3933
_journal_paper_doi               10.1021/ic102226j
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C21 H29 Cu2 N11 O1, 0.5(C3 H7 N O)'
_chemical_formula_sum            'C22.5 H32.5 Cu2 N11.5 O1.5'
_chemical_formula_weight         615.18
_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                 103.887(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.6314(10)
_cell_length_b                   16.5650(10)
_cell_length_c                   19.2469(11)
_cell_measurement_temperature    293(2)
_cell_volume                     5457.0(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37353
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    1.600
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       Block
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         6493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0618P)^2^+5.1587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1186
_reflns_number_gt                4523
_reflns_number_total             6493
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic102226j_si_001_2.cif
_cod_data_source_block           DR-MS-1-769535
_cod_original_cell_volume        5457.0(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C22.50 H32.50 Cu2 N11.50 O1.50'
_cod_database_code               4324942