Field-induced slow magnetic relaxation in mixed valence di- and tri-nuclear Co<sup>II</sup>-Co<sup>III</sup> complexes.
Paul, Aparup; Viciano-Chumillas, Marta; Puschmann, Horst; Cano, Joan; Manna, Subal Chandra; Dalton transactions (Cambridge, England : 2003) 49 (2020) 9516–9528; doi:10.1039/d0dt00588f

data_7704677
_publ_section_title
;
 Field-induced slow magnetic relaxation in mixed valence di- and
 tri-nuclear Co<sup>II</sup>-Co<sup>III</sup> complexes.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9516
_journal_page_last               9528
_journal_paper_doi               10.1039/d0dt00588f
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C44 H52 Co3 N4 O20, 2(H2 O)'
_chemical_formula_sum            'C44 H56 Co3 N4 O22'
_chemical_formula_weight         1169.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-03-07
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2017.02.02 svn.r3383 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2020-01-27 deposited with the CCDC.	2020-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.509(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7106(5)
_cell_length_b                   9.7609(6)
_cell_length_c                   35.2338(14)
_cell_measurement_reflns_used    6496
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.5740
_cell_measurement_theta_min      2.1560
_cell_volume                     4684.9(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.38.7t (release 04-09-2014 CrysAlis171 .NET)
(compiled Sep  4 2014,14:28:23)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.38.7t (release 04-09-2014 CrysAlis171 .NET)
(compiled Sep  4 2014,14:28:23)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.38.7t (release 04-09-2014 CrysAlis171 .NET)
(compiled Sep  4 2014,14:28:23)
;
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0756
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -24.00   22.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.1554 -100.0000  150.0000 46

  2 omega  -24.00   22.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.1554 -100.0000    0.0000 46

  3 omega  -24.00   22.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.1554 -100.0000  -90.0000 46

  4 omega   -5.00   93.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9366   38.0000 -180.0000 98

  5 omega   35.00   97.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9366  178.0000   60.0000 62

  6 omega    0.00   90.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9366   57.0000  -90.0000 90

  7 omega  -23.00   94.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9366   19.0000  -60.0000 117

  8 omega  -51.00   46.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9366  -38.0000    0.0000 97

  9 omega  -96.00  -35.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.1554 -178.0000   90.0000 61

 10 omega  -48.00   42.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9366  -57.0000 -120.0000 90

 11 omega  -24.00   29.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9366 -100.0000  120.0000 53

 12 omega    0.00   90.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9366   57.0000   30.0000 90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0031194000
_diffrn_orient_matrix_UB_12      -0.0549300000
_diffrn_orient_matrix_UB_13      0.0132737000
_diffrn_orient_matrix_UB_21      0.0182270000
_diffrn_orient_matrix_UB_22      0.0456728000
_diffrn_orient_matrix_UB_23      0.0147908000
_diffrn_orient_matrix_UB_31      -0.0486530000
_diffrn_orient_matrix_UB_32      0.0135190000
_diffrn_orient_matrix_UB_33      0.0039347000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1130
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            34583
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         2.166
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           35
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.303
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.38.7t (release 04-09-2014 CrysAlis171 .NET)
(compiled Sep  4 2014,14:28:23)
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            'dull dark brown'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       plate
_exptl_crystal_F_000             2420
_exptl_crystal_recrystallization_method
'The material was recrystallised from water by slow evaporation'
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.526
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         4120
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0330P)^2^+11.8780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3567
_reflns_number_total             4120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00588f2.cif
_cod_data_source_block           icvu_243
_cod_depositor_comments
'Adding full bibliography for 7704677--7704678.cif.'
_cod_original_cell_volume        4684.8(4)
_cod_database_code               7704677
_shelx_shelxl_version_number     2016/6
_audit_section_references
;
Bourhis, L.J., Dolomanov, O.V., Gildea, R.J., Howard, J.A.K., Puschmann, H.
 (2013). in preparation.

Bourhis, L.J., Dolomanov, O.V., Gildea, R.J., Howard, J.A.K., Puschmann, H.
 (2015). Acta Cryst. A71, 59-75.

Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_oxdiff_formula         C44H56Co3N4O22
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, All O(H,H) groups
2. Rigid body (RIGU) restrains
 O22, O21, C21, Co1, O23, C22, O12, N11, N21, O11, Co2, C23, C210, C110, C13,
 C14, C24, C11, O2W, O1W, C25, C29, C15, C19, C12, O13, C26, O24, C28, C16, O14,
  C18, C27, C211, C17, C111
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Free rotating group:
 O3W(H3WA,H3WB)
3.b Rotating group:
 O2W(H2WA,H2WB), O1W(H1WA,H1WB)
3.c Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B), C12(H12A,H12B), C13(H13A,H13B)
3.d Aromatic/amide H refined with riding coordinates:
 C24(H24), C28(H28), C27(H27), C26(H26), C14(H14), C18(H18), C17(H17), C16(H16)
3.e Idealised Me refined as rotating group:
 C211(H21A,H21B,H21C), C111(H11A,H11B,H11C)
;
_shelx_res_checksum              25162
_olex2_date_sample_data_collection 2015-01-26
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems 700 Plus Series'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a hair in perfluoroether oil'
_olex2_submission_original_sample_id ICVU_243
_olex2_submission_special_instructions 'No special instructions were received'