Relaxation Dynamics of Identical Trigonal Bipyramidal Cobalt Molecules with Different Local Symmetries and Packing Arrangements: Magnetostructural Correlations and ab inito Calculations.
Woods, Toby J.; Ballesteros-Rivas, María F; Gómez-Coca, Silvia; Ruiz, Eliseo; Dunbar, Kim R.; Journal of the American Chemical Society 138 (2016) 16407–16416; doi:10.1021/jacs.6b10154

data_4131139
_publ_section_title
;
 Relaxation Dynamics of Identical Trigonal Bipyramidal Cobalt Molecules
 with Different Local Symmetries and Packing Arrangements:
 Magnetostructural Correlations and ab inito Calculations.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16407
_journal_page_last               16416
_journal_paper_doi               10.1021/jacs.6b10154
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety
'C18 H18 Br Co N4, 0.81(Br), 0.17(Br0.56 O0.82), 0.33(Br0.3 O0.86), 1.58(O)'
_chemical_formula_sum            'C18 H18 Br2 Co N4 O2'
_chemical_formula_weight         541.11
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90.7760(10)
_cell_angle_beta                 102.8730(10)
_cell_angle_gamma                110.7960(10)
_cell_formula_units_Z            6
_cell_length_a                   11.7529(4)
_cell_length_b                   15.0871(5)
_cell_length_c                   20.3000(7)
_cell_measurement_reflns_used    48434
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.35
_cell_measurement_theta_min      3.68
_cell_volume                     3263.46(19)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2 v2014.11-0'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Diamond v3.2i'
_computing_publication_material  'SHELXL-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/5 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            97930
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.746
_diffrn_reflns_theta_min         2.244
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.651
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014) was used for absorption correction. wR2(int) was 0.1229 before and 0.0627 after correction. The Ratio of minimum to maximum transmission is 0.6449. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       plate
_exptl_crystal_F_000             1602
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.035
_refine_diff_density_max         2.290
_refine_diff_density_min         -1.724
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         11855
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0973P)^2^+24.1751P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1817
_refine_ls_wR_factor_ref         0.1951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10094
_reflns_number_total             11855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b10154_si_002.cif
_cod_data_source_block           autop_1_a_CoTPMABr_triclinic
_cod_database_code               4131139
_shelxl_version_number           2014/5
_shelx_estimated_absorpt_t_max   0.707
_shelx_estimated_absorpt_t_min   0.321
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Br5) = Uanis(Br6) = Uanis(Br7) = Uanis(Br8) = Uanis(Br9) = Uanis(Br10)
Uanis(O1) = Uanis(O2) = Uanis(O3) = Uanis(O4) = Uanis(O5) = Uanis(O6) =
Uanis(O7) = Uanis(O8) = Uanis(O9)
3. Others
 1*[Sof(Br5)]+1*[Sof(Br6)]+1*[Sof(Br7)]+1*[Sof(Br8)]+1*[Sof(Br9)]+1*
 [Sof(Br10)]=2 with esd of 0.001
 1*[Sof(O1)]+1*[Sof(O2)]+1*[Sof(O3)]+1*[Sof(O4)]+1*[Sof(O5)]+1*[Sof(O6)]+1*
 [Sof(O7)]+1*[Sof(O8)]+1*[Sof(O9)]=6 with esd of 0.001
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B), C19(H19A,H19B), C25(H25A,H25B),
 C31(H31A,H31B), C37(H37A,H37B), C43(H43A,H43B), C49(H49A,H49B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C27(H27), C24(H24), C23(H23),
  C22(H22), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34), C35(H35),
 C36(H36), C39(H39), C40(H40), C41(H41), C42(H42), C45(H45), C46(H46), C47(H47),
  C48(H48), C51(H51), C52(H52), C53(H53), C54(H54)
;
_shelx_res_checksum              31455
_shelx_hkl_checksum              76496
_olex2_submission_special_instructions 'No special instructions were received'