Redox-switchable tetra-copper assembly of N,N-, N,O-phenolate-phenanthroimidazolate bridging ligands.
Mathias, Jenny-Lee; Arora, Himanshu; Lavi, Ronit; Vezin, Hervé; Yufit, Dmitry; Orio, Maylis; Aliaga-Alcade, Núria; Benisvy, Laurent; Dalton transactions (Cambridge, England : 2003) 42 (2013) 2358–2361; doi:10.1039/c2dt32585c

data_7020946
_publ_section_title
;
 Redox-switchable tetra-copper assembly of N,N-,
 N,O-phenolate-phenanthroimidazolate bridging ligands.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2358
_journal_page_last               2361
_journal_paper_doi               10.1039/c2dt32585c
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C108 H104 Cu4 N16 O4, 10(C2 H3 N), H2 O'
_chemical_formula_sum            'C128 H136 Cu4 N26 O5'
_chemical_formula_weight         2372.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-07-03
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                100.234(10)
_cell_angle_beta                 102.677(10)
_cell_angle_gamma                116.684(10)
_cell_formula_units_Z            2
_cell_length_a                   18.2124(7)
_cell_length_b                   19.5173(8)
_cell_length_c                   21.1956(8)
_cell_measurement_reflns_used    7675
_cell_measurement_temperature    120
_cell_measurement_theta_max      26.69
_cell_measurement_theta_min      2.24
_cell_volume                     6229.2(10)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.1626
_diffrn_reflns_av_unetI/netI     0.1901
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            91291
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.27
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.737
_exptl_absorpt_correction_T_max  0.8879
_exptl_absorpt_correction_T_min  0.4395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2006/1 (Bruker,2006) was used for absorption correction.
R(int) was 0.0688 before and 0.0469 after correction.
The Ratio of minimum to maximum transmission is 0.4950.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2492
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.246
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1473
_refine_ls_number_reflns         30032
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.1819
_refine_ls_R_factor_gt           0.0653
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1787
_reflns_number_gt                12998
_reflns_number_total             30032
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt32585c.txt
_cod_data_source_block           (I_CH3CN)_dbl14a
_cod_original_cell_volume        6229.2(4)
_cod_database_code               7020946