Room-Temperature Characterization of a Mixed-Valent μ-Hydroxodicopper(II,III) Complex.
Isaac, James A.; Gennarini, Federica; López, Isidoro; Thibon-Pourret, Aurore; David, Rolf; Gellon, Gisèle; Gennaro, Béatrice; Philouze, Christian; Meyer, Franc; Demeshko, Serhiy; Le Mest, Yves; Réglier, Marius; Jamet, Hélène; Le Poul, Nicolas; Belle, Catherine; Inorganic chemistry 55 (2016) 8263–8266; doi:10.1021/acs.inorgchem.6b01504

data_4348665
_publ_section_title
;
 Room-Temperature Characterization of a Mixed-Valent
 \m-Hydroxodicopper(II,III) Complex.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8263
_journal_page_last               8266
_journal_paper_doi               10.1021/acs.inorgchem.6b01504
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety
'C32 H28 Cu2 N6 O2, 2(C F3 O3 S), 1.8(C2 H3 N)'
_chemical_formula_sum            'C37.62 H33.42 Cu2 F6 N7.81 O8 S2'
_chemical_formula_weight         1028.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-07-20
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                70.13(3)
_cell_angle_beta                 68.96(3)
_cell_angle_gamma                76.69(3)
_cell_formula_units_Z            4
_cell_length_a                   14.783(3)
_cell_length_b                   17.300(4)
_cell_length_c                   18.904(4)
_cell_measurement_reflns_used    82271
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.49
_cell_volume                     4211.3(19)
_computing_cell_refinement       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            KappaCCD
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-AXS-enraf-nonius KappaCCD'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_collimation    'Montel optic'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            82271
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.487
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    1.197
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.666378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction. R(int)
 was 0.1474 before and 0.0395 after correction. The Ratio of minimum
 to maximum transmission is 0.6664. The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2087
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.456
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1279
_refine_ls_number_reflns         19295
_refine_ls_number_restraints     451
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0382P)^2^+14.4085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1478
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10403
_reflns_number_total             19295
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01504_si_002.cif
_cod_data_source_block           nanny
_cod_original_cell_volume        4211.3(15)
_cod_database_code               4348665
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C33"-S1A
 1.8 with sigma of 0.02
 S1A'-C33A
 1.8 with sigma of 0.02
 F1A-C33"
 1.33 with sigma of 0.02
 C33"-F2A
 1.33 with sigma of 0.02
 C33A-F3A'
 1.33 with sigma of 0.02
 C33A-F2A'
 1.33 with sigma of 0.02
 C33"-F3A
 1.33 with sigma of 0.02
 C33A-F1A'
 1.33 with sigma of 0.02
 F1A'-F3A'
 2.1 with sigma of 0.02
 F3A'-F2A'
 2.1 with sigma of 0.02
 F1A'-F2A'
 2.1 with sigma of 0.02
 F1A-F3A
 2.1 with sigma of 0.02
 F1A-F2A
 2.1 with sigma of 0.02
 F2A-F3A
 2.1 with sigma of 0.02
 C33'-F2B'
 1.33 with sigma of 0.02
 F3B'-C33'
 1.33 with sigma of 0.02
 F2B'-F3B'
 2.1 with sigma of 0.02
 F1B'-F2B'
 2.1 with sigma of 0.02
 F3B'-F1B'
 2.1 with sigma of 0.02
 C33'-F1B'
 1.33 with sigma of 0.02
 S1B'-F1B'
 2.6 with sigma of 0.02
 S1B'-F3B'
 2.6 with sigma of 0.02
 S1B'-F2B'
 2.6 with sigma of 0.02
 O5B'-O4B'
 2.42 with sigma of 0.02
 O4B'-O3B'
 2.42 with sigma of 0.02
 O4B-O5B
 2.42 with sigma of 0.02
 O5B-O3B
 2.42 with sigma of 0.02
 O3B-O4B
 2.42 with sigma of 0.02
 O4B'-S1B'
 1.42 with sigma of 0.02
 O3B'-S1B'
 1.42 with sigma of 0.02
 S1B'-O5B'
 1.42 with sigma of 0.02
 O3A-C33A = C33'-O5B'
 2.7 with sigma of 0.02
3. Rigid bond restraints
 F3A, O3A, S1A, S1A', O5A, O4A, C33", O5A', O4A', C33A, F1A, F2A, F2A', F3A',
 F1A'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O5B', O3B', S1B', C33', O4B', F2B', F3B', F1B', O3B, S1B, O5B, C33B, O4B, F2B,
  F3B, F1B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F3A \\sim O3A \\sim S1A \\sim S1A' \\sim O5A \\sim O4A \\sim C33" \\sim O5A'
\\sim O4A' \\sim C33A \\sim F1A \\sim F2A \\sim F2A' \\sim F3A' \\sim F1A':
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
O4B' \\sim O3B' \\sim S1B' \\sim O5B' \\sim C33' \\sim F2B' \\sim F3B' \\sim
F1B' \\sim O3B \\sim S1B \\sim O5B \\sim C33B \\sim O4B \\sim F2B \\sim F3B
\\sim F1B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O4B') = Uanis(O4B)
Uanis(F3B') = Uanis(F3B)
Uanis(C33') = Uanis(C33B)
Uanis(F2B) = Uanis(F2B')
5. Others
 Sof(S1A')=Sof(O5A')=Sof(O4A')=Sof(C33A)=Sof(F2A')=Sof(F3A')=Sof(F1A')=1-FVAR(1)
 Sof(S1A)=Sof(O5A)=Sof(O4A)=Sof(F1A)=Sof(F2A)=Sof(C33")=Sof(F3A)=FVAR(1)
 Sof(N3)=Sof(C35B)=Sof(C36B)=Sof(H36D)=Sof(H36E)=Sof(H36F)=FVAR(2)
 Sof(O3B')=Sof(O5B')=Sof(S1B')=Sof(F2B')=Sof(F3B')=Sof(C33')=Sof(O4B')=
 Sof(F1B')=1-FVAR(3)
 Sof(S1B)=Sof(O5B)=Sof(F2B)=Sof(F3B)=Sof(F1B)=Sof(C33B)=Sof(O4B)=Sof(O3B)=
 FVAR(3)
6.a Rotating group:
 O2A(H2A), O1A(H1A), O1B(H1B), O2B(H2B)
6.b Aromatic/amide H refined with riding coordinates:
 C23A(H23A), C2A(H2AA), C19B(H19B), C18A(H18A), C2B(H2BA), C3A(H3A), C7B(H7B),
 C3B(H3B), C30B(H30B), C7A(H7A), C6A(H6A), C14A(H14A), C13B(H13B), C28B(H28B),
 C31B(H31B), C31A(H31A), C26A(H26A), C23B(H23B), C29A(H29A), C28A(H28A),
 C24B(H24B), C6B(H6B), C29B(H29B), C30A(H30A), C16B(H16B), C24A(H24A),
 C11A(H11A), C26B(H26B), C17B(H17B), C18B(H18B), C25A(H25A), C17A(H17A),
 C25B(H25B), C16A(H16A), C19A(H19A), C12B(H12B), C11B(H11B), C13A(H13A),
 C12A(H12A), C14B(H14B)
6.c Idealised Me refined as rotating group:
 C32B(H32D,H32E,H32F), C32A(H32A,H32B,H32C), C20A(H20A,H20B,H20C), C20B(H20D,
 H20E,H20F), C36A(H36A,H36B,H36C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C),
 C36B(H36D,H36E,H36F)
;
_shelx_res_checksum              26690
_shelx_hkl_checksum              45571
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'