On the magneto-structural role of the coordinating anion in oxamato-bridged copper(ii) derivatives.
Simões, Tatiana R G; Marinho, Maria Vanda; Pasán, Jorge; Stumpf, Humberto O.; Moliner, Nicolás; Lloret, Francesc; Julve, Miguel; Dalton transactions (Cambridge, England : 2003) 48 (2019) 10260–10274; doi:10.1039/c9dt01277j

data_7700191
_publ_section_title
;
 On the magneto-structural role of the coordinating anion in
 oxamato-bridged copper(ii) derivatives.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10260
_journal_page_last               10274
_journal_paper_doi               10.1039/c9dt01277j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C40 H28 Cu3 N8 O7 S2, C3 H7 N O, 0.20(O)'
_chemical_formula_sum            'C43 H35 Cu3 N9 O8.2 S2'
_chemical_formula_weight         1063.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-05-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-22 deposited with the CCDC.    2019-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.411(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4163(4)
_cell_length_b                   21.8732(12)
_cell_length_c                   10.9475(5)
_cell_measurement_reflns_used    3791
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.1140
_cell_measurement_theta_min      1.8310
_cell_volume                     2254.11(19)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1268
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, EosS2'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12516
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.284
_diffrn_reflns_theta_min         1.862
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.558
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       prism
_exptl_crystal_F_000             1081
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5175
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+1.6999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3999
_reflns_number_total             5175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01277j2.cif
_cod_data_source_block           compound_1
_cod_depositor_comments
'Adding full bibliography for 7700191--7700194.cif.'
_cod_original_formula_sum        'C43 H35 Cu3 N9 O8.20 S2'
_cod_database_code               7700191
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C20-S1 \\sim C20A-S1A
 with sigma of 0.02
 N4-C20 \\sim N4A-C20A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N4A) = Uanis(N4)
Uanis(C20A) = Uanis(C20)
4. Rigid body (RIGU) restrains
 S1, N4, C20, S1A, N4A, C20A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S1A)=Sof(N4A)=Sof(C20A)=1-FVAR(1)
 Sof(S1)=Sof(N4)=Sof(C20)=FVAR(1)
 Fixed Sof: H22A(0.5) H22B(0.5) H22C(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C14(H14),
 C21(H21)
6.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C)
;
_shelx_res_checksum              74471
_olex2_submission_special_instructions 'No special instructions were received'