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_7048098
_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
_chemical_melting_point          ?
_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-2016/6
_audit_update_record
;
2018-09-03 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.607(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1426(14)
_cell_length_b                   15.8923(14)
_cell_length_c                   17.1821(15)
_cell_measurement_reflns_used    9205
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.50
_cell_measurement_theta_min      2.40
_cell_volume                     4346.1(7)
_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-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0420
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            154061
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.724
_diffrn_reflns_theta_min         1.757
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.022
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2196
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DMF, ether'
_exptl_crystal_size_max          0.87
_exptl_crystal_size_mid          0.78
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.788
_refine_diff_density_min         -1.812
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         11240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0752P)^2^+8.8092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1427
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8787
_reflns_number_total             11240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03833c2.cif
_cod_data_source_block           3-Et2O-298K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7048090--7048108.cif.
;
_cod_database_code               7048098
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.179
_shelx_estimated_absorpt_t_max   0.350
_shelx_res_checksum              46504