Interactions between H-bonded [Cu(μ<sub>3</sub>-OH)] triangles; a combined magnetic susceptibility and EPR study.
Mathivathanan, Logesh; Boudalis, Athanassios K.; Turek, Philippe; Pissas, Michael; Sanakis, Yiannis; Raptis, Raphael G.; Physical chemistry chemical physics : PCCP 20 (2018) 17234–17244; doi:10.1039/c8cp02643b

data_7230888
_publ_section_title
;
 Interactions between H-bonded [Cu(\m<sub>3</sub>-OH)] triangles; a
 combined magnetic susceptibility and EPR study.
;
_journal_issue                   25
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              17234
_journal_page_last               17244
_journal_paper_doi               10.1039/c8cp02643b
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C30 H25 Cu3 N6 O7, H2 O, C6 H16 N'
_chemical_formula_sum            'C36 H43 Cu3 N7 O8'
_chemical_formula_weight         892.39
_chemical_name_systematic
'triethylammonium (m3-hydroxido)(tris-m-pyrazolido)tribenzoato tricopper(II)'
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-22 deposited with the CCDC.
2018-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                73.446(2)
_cell_angle_beta                 79.252(2)
_cell_angle_gamma                65.891(2)
_cell_formula_units_Z            2
_cell_length_a                   11.417(2)
_cell_length_b                   12.317(3)
_cell_length_c                   15.889(3)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.22
_cell_measurement_theta_min      2.18
_cell_volume                     1948.6(7)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22341
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.457
_diffrn_reflns_theta_min         1.960
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.681
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1251 before and 0.0339 after correction. The Ratio of minimum to maximum transmission is 0.9257. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       Polygon
_exptl_crystal_F_000             918
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: CH3CN'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8671
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0477P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0867
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6433
_reflns_number_total             8671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cp02643b2.cif
_cod_data_source_block           log120_0m
_cod_depositor_comments          'Adding full bibliography for 7230888.cif.'
_cod_original_cell_volume        1948.7(7)
_cod_database_code               7230888
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.877
_shelx_estimated_absorpt_t_min   0.799
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O8-H8B = O8-H8A
 1 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C33(H33A,H33B), C35(H35A,H35B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30)
3.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              68490
_olex2_submission_special_instructions 'No special instructions were received'