Temperature dependence of the spin state and geometry in tricobalt paddlewheel complexes with halide axial ligands.
Srinivasan, Anandi; Wang, Xiaoping; Clérac, Rodolphe; Rouzières, Mathieu; Falvello, Larry R.; McGrady, John E.; Hillard, Elizabeth A.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 16798–16806; doi:10.1039/c8dt03833c

data_7048107
_publ_section_title
;
 Temperature dependence of the spin state and geometry in tricobalt
 paddlewheel complexes with halide axial ligands.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16798
_journal_page_last               16806
_journal_paper_doi               10.1039/c8dt03833c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C40 H32 Br2 Co3 N12, C4 H10 O'
_chemical_formula_sum            'C44 H42 Br2 Co3 N12 O'
_chemical_formula_weight         1091.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-11-05 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.293(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1914(13)
_cell_length_b                   15.9355(12)
_cell_length_c                   17.2266(14)
_cell_measurement_reflns_used    9695
_cell_measurement_temperature    350(2)
_cell_measurement_theta_max      26.72
_cell_measurement_theta_min      2.28
_cell_volume                     4386.4(6)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'WinGX (Farrugia, 2012)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      350(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0576
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            137516
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.528
_diffrn_reflns_theta_min         1.752
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.994
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.3767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2196
_exptl_crystal_size_max          0.544
_exptl_crystal_size_mid          0.403
_exptl_crystal_size_min          0.238
_refine_diff_density_max         0.756
_refine_diff_density_min         -1.718
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         10059
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0758P)^2^+12.1275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1579
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7734
_reflns_number_total             10059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03833c2.cif
_cod_data_source_block           3-et2o-350k
_cod_depositor_comments
'Adding full bibliography for 7048090--7048108.cif.'
_cod_database_code               7048107
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.293
_shelx_estimated_absorpt_t_max   0.536
_shelx_res_checksum              8145