Oxalate-based [CuIICrIII] coordination compounds affected by the tridentate ligand, simple anion, and reactant ratio: structural and magnetic features
Molčanov, Lidija; Šenjug, Pavla; Barišić, Dario; Pajić, Damir; Molčanov, Krešimir; Jurić, Marijana; Dalton Transactions  (2022) –; doi:10.1039/D2DT01949C

data_7711455
_publ_section_title
;
 Oxalate-based [CuIICrIII] coordination compounds affected by the
 tridentate ligand, simple anion, and reactant ratio: structural and
 magnetic features
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01949C
_journal_year                    2022
_chemical_formula_moiety
'C60 H44 Cl5 Cu4 N12, C6 Cr O12, 7.67(H2 O), 0.33(O)'
_chemical_formula_sum            'C66 H68 Cl5 Cr Cu4 N12 O24'
_chemical_formula_weight         1896.73
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-08-22 deposited with the CCDC.	2022-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                81.878(2)
_cell_angle_beta                 78.234(2)
_cell_angle_gamma                83.750(3)
_cell_formula_units_Z            2
_cell_length_a                   12.7176(4)
_cell_length_b                   15.2066(5)
_cell_length_c                   20.0501(5)
_cell_measurement_reflns_used    24023
_cell_measurement_temperature    159.9(3)
_cell_measurement_theta_max      32.0680
_cell_measurement_theta_min      2.5290
_cell_volume                     3745.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_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_environment      N~2~
_diffrn_ambient_temperature      159.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4498
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -25.00  21.40   0.80   25.00    --  -18.05 -99.00 -30.00   58
  2  \w     -8.00  88.00   0.80   25.00    --   18.99  57.00-150.00  120
  3  \w     35.00 105.40   0.80   25.00    --   18.99 178.00  90.00   88
  4  \w     -8.00  88.00   0.80   25.00    --   18.99  57.00 -30.00  120
  5  \w    -51.00  45.00   0.80   25.00    --   18.99 -57.00  60.00  120
  6  \w    -77.00 -31.40   0.80   25.00    --  -18.05 132.00 -57.00   57
  7  \w    -25.00  21.40   0.80   25.00    --  -18.05 -99.00  60.00   58
  8  \w    -25.00  59.00   0.80   25.00    --   18.99 -99.00-180.00  105
  9  \w    -12.00  92.00   0.80   25.00    --   18.99  77.00  60.00  130
 10  \w    -54.00  42.00   0.80   25.00    --   18.99 -38.00-120.00  120
 11  \w    -51.00  45.00   0.80   25.00    --   18.99 -57.00-150.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0206807000
_diffrn_orient_matrix_UB_12      -0.0450590000
_diffrn_orient_matrix_UB_13      -0.0015604000
_diffrn_orient_matrix_UB_21      0.0085954000
_diffrn_orient_matrix_UB_22      0.0073803000
_diffrn_orient_matrix_UB_23      -0.0363614000
_diffrn_orient_matrix_UB_31      0.0525960000
_diffrn_orient_matrix_UB_32      0.0122664000
_diffrn_orient_matrix_UB_33      -0.0010256000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            102921
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.385
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.522
_exptl_absorpt_correction_T_max  0.861
_exptl_absorpt_correction_T_min  0.741
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_description       prism
_exptl_crystal_F_000             1930
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.754
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1009
_refine_ls_number_reflns         22874
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+2.4839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1108
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15799
_reflns_number_total             22874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01949c2.cif
_cod_data_source_block           p53
_cod_database_code               7711455
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C66 H68 Cl5 Cr Cu4 N12 O24'
_chemical_oxdiff_usercomment     'Lidija Kanizaj ZSC'
_shelx_estimated_absorpt_t_max   0.850
_shelx_estimated_absorpt_t_min   0.675
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O10B-C0 = O10A-C3 = O9A-C2 = O9B-C1
 1.28 with sigma of 0.02
 O11B-C0 \\sim O11A-C3 \\sim O12B-C1 \\sim O12A-C2
 with sigma of 0.02
 C1-C0 \\sim C3-C2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O25) = Uanis(O26)
4. Others
 Sof(OW7B)=Sof(HW7C)=Sof(HW7D)=1-FVAR(1)
 Sof(OW7A)=Sof(HW7A)=Sof(HW7B)=FVAR(1)
 Sof(O26)=1-FVAR(2)
 Sof(O25)=Sof(H25A)=Sof(H25B)=FVAR(2)
 Sof(O10B)=Sof(O9B)=Sof(O11B)=Sof(C0)=Sof(O12B)=Sof(C1)=1-FVAR(3)
 Sof(O12A)=Sof(C2)=Sof(C3)=Sof(O11A)=Sof(O9A)=Sof(O10A)=FVAR(3)
5.a Free rotating group:
 OW3(HW3A,HW3B), OW2(HW2A,HW2B), OW1(HW1A,HW1B), OW4(HW4A,HW4B), OW5(HW5A,
 HW5B), OW6(HW6A,HW6B), O25(H25A,H25B), OW7A(HW7A,HW7B), OW7B(HW7C,HW7D)
5.b Aromatic/amide H refined with riding coordinates:
 C013(H013), C018(H018), C019(H019), C01D(H01D), C01I(H01I), C01J(H01J),
 C01K(H01K), C01L(H01L), C01M(H01M), C01N(H01N), C01P(H01P), C01Q(H01Q),
 C01S(H01S), C01W(H01W), C01Z(H01Z), C022(H022), C023(H023), C024(H024),
 C025(H025), C026(H026), C027(H027), C028(H028), C029(H029), C02A(H02A),
 C02C(H02C), C02E(H02E), C02F(H02F), C02G(H02G), C02H(H02H), C02J(H02J),
 C02L(H02L), C02M(H02M), C02N(H02N), C02P(H02P), C02Q(H02Q), C02R(H02R),
 C02S(H02S), C02T(H02T), C02U(H02U), C02V(H02V), C02W(H02W), C02Y(H02Y),
 C02Z(H02Z), C030(H030)
;
_shelx_res_checksum              35435
_shelx_hkl_checksum              89962
_shelx_fab_checksum              89223
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.129
_oxdiff_exptl_absorpt_empirical_full_min 0.847