Slow magnetic relaxation in a {Co<sup>II</sup>Co} complex containing a high magnetic anisotropy trigonal bipyramidal Co<sup>II</sup> centre.
Collet, Alexandra; Craig, Gavin A.; Heras Ojea, María José; Bhaskaran, Lakshmi; Wilson, Claire; Hill, Stephen; Murrie, Mark; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9237–9240; doi:10.1039/c8dt01997e

data_7046700
_publ_section_title
;
 Slow magnetic relaxation in a {Co<sup>II</sup>Co} complex containing a
 high magnetic anisotropy trigonal bipyramidal Co<sup>II</sup> centre.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9237
_journal_page_last               9240
_journal_paper_doi               10.1039/c8dt01997e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C57 H46 Co3 N8 O7, 2(C2 H3 N)'
_chemical_formula_sum            'C61 H52 Co3 N10 O7'
_chemical_formula_weight         1213.91
_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
_audit_creation_date             2016-04-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-04-19 deposited with the CCDC.
2018-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                85.880(19)
_cell_angle_beta                 71.750(19)
_cell_angle_gamma                72.444(18)
_cell_formula_units_Z            2
_cell_length_a                   13.250(10)
_cell_length_b                   14.173(11)
_cell_length_c                   16.426(13)
_cell_measurement_reflns_used    9395
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.10
_cell_measurement_theta_min      2.44
_cell_volume                     2792(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       COLLECT
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      100
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0800
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15656
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.162
_diffrn_reflns_theta_min         1.794
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0644 before and 0.0524 after correction.
 The Ratio of minimum to maximum transmission is 0.79.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1039 before and 0.0715 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 66673 reflections, Rint = 0.0639
 (31306 with I > 3sig(I), Rint = 0.0490)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       column
_exptl_crystal_F_000             1250
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         9616
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0453P)^2^+1.4852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1108
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6683
_reflns_number_total             9616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01997e2.cif
_cod_data_source_block           1_2MeCN
_cod_depositor_comments          'Adding full bibliography for 7046700.cif.'
_cod_database_code               7046700
_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
 O1-H1
 0.84 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C18(H18), C19(H19), C20(H20), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A),
  C7A(H7A), C8A(H8A), C11A(H11A), C12A(H12A), C13A(H13A), C14A(H14A),
 C15A(H15A), C3B(H3B), C4B(H4B), C5B(H5B), C6B(H6B), C7B(H7B), C8B(H8B),
 C11B(H11B), C12B(H12B), C13B(H13B), C14B(H14B), C15B(H15B), C3C(H3C), C4C(H4C),
  C5C(H5C), C6C(H6C), C7C(H7C), C8C(H8C), C11C(H11C), C12C(H12C), C13C(H13C),
 C14C(H14C), C15C(H15C)
3.b Idealised Me refined as rotating group:
 C3S(H3SA,H3SB,H3SC), C6S(H6SA,H6SB,H6SC)
;
_shelx_res_checksum              3587
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'