Valence tautomerism and spin crossover in pyridinophane-cobalt-dioxolene complexes: an experimental and computational study.
Tezgerevska, Tina; Rousset, Elodie; Gable, Robert W.; Jameson, Guy N. L.; Sañudo, E Carolina; Starikova, Alyona; Boskovic, Colette; Dalton transactions (Cambridge, England : 2003) 48 (2019) 11674–11689; doi:10.1039/c9dt02372k

data_7700424
_publ_section_title
;
 Valence tautomerism and spin crossover in pyridinophane-cobalt-dioxolene
 complexes: an experimental and computational study.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11674
_journal_page_last               11689
_journal_paper_doi               10.1039/c9dt02372k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C32 H44 Co N4 O2, C24 H20 B, 2(C4 H8 O2)'
_chemical_formula_sum            'C64 H80 B Co N4 O6'
_chemical_formula_weight         1071.06
_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   geom
_audit_creation_date             2018-09-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-29 deposited with the CCDC.    2019-07-02 downloaded from the CCDC.
;
_cell_angle_alpha                95.654(3)
_cell_angle_beta                 92.389(3)
_cell_angle_gamma                99.975(3)
_cell_formula_units_Z            2
_cell_length_a                   11.0684(4)
_cell_length_b                   11.8545(4)
_cell_length_c                   22.1063(8)
_cell_measurement_reflns_used    8910
_cell_measurement_temperature    130.00(10)
_cell_measurement_theta_max      73.7910
_cell_measurement_theta_min      4.0240
_cell_volume                     2837.72(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      130.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -114.00 -14.00   1.00    6.00    --  -41.87 -57.00 -60.00  100
  2  \w    -29.00  -3.00   1.00    6.00    --  -41.87 125.00  60.00   26
  3  \w    -46.00  24.00   1.00    6.00    --  -41.87  38.00-120.00   70
  4  \w    -49.00  32.00   1.00    6.00    --  -41.87  38.00  90.00   81
  5  \w     14.00  58.00   1.00    6.00    --   41.87 -99.00 150.00   44
  6  \w     41.00  97.00   1.00    6.00    --   41.87-125.00 -60.00   56
  7  \w     26.00  87.00   1.00   30.00    --  105.57 -94.00 -30.00   61
  8  \w     24.00 109.00   1.00   30.00    --  105.57 -94.00 150.00   85
  9  \w     66.00  93.00   1.00   30.00    --  105.57 -45.00 120.00   27
 10  \w     45.00  73.00   1.00   30.00    --  105.57 -30.00  30.00   28
 11  \w     93.00 173.00   1.00   30.00    --  105.57  30.00   0.00   80
 12  \w    103.00 129.00   1.00   30.00    --  105.57 -61.00-120.00   26
 13  \w     36.00  94.00   1.00   30.00    --  105.57 -94.00-120.00   58
 14  \w     32.00 118.00   1.00   30.00    --  105.57-125.00 120.00   86
 15  \w     29.00  89.00   1.00   30.00    --  105.57 -30.00 -30.00   60
 16  \w     34.00  83.00   1.00   30.00    --  105.57 -61.00-120.00   49
 17  \w     51.00  86.00   1.00   30.00    --  105.57 -30.00  90.00   35
 18  \w     51.00  88.00   1.00   30.00    --  105.57 -94.00  30.00   37
 19  \w     90.00 118.00   1.00   30.00    --  105.57-125.00   0.00   28
 20  \w     54.00 177.00   1.00   30.00    --  105.57  15.00 -60.00  123
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0858850000
_diffrn_orient_matrix_UB_12      -0.1041570000
_diffrn_orient_matrix_UB_13      -0.0350981000
_diffrn_orient_matrix_UB_21      0.0854713000
_diffrn_orient_matrix_UB_22      0.0048922000
_diffrn_orient_matrix_UB_23      -0.0532871000
_diffrn_orient_matrix_UB_31      0.0732271000
_diffrn_orient_matrix_UB_32      -0.0821078000
_diffrn_orient_matrix_UB_33      0.0291620000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20930
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.070
_diffrn_reflns_theta_min         3.808
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.802
_exptl_absorpt_correction_T_max  0.846
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone, dioxane'
_exptl_crystal_size_max          0.363
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.093
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     693
_refine_ls_number_reflns         11189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0580P)^2^+0.6293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1041
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10427
_reflns_number_total             11189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02372k3.cif
_cod_data_source_block           2-co
_cod_depositor_comments
'Adding full bibliography for 7700424--7700427.cif.'
_cod_database_code               7700424
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C64H79BCoN4O6
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C21(H21A,H21B), C22(H22A,H22B), C28(H28A,H28B), C29(H29A,
 H29B), C31(H31A,H31B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B),
 C64(H64A,H64B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C17(H17), C18(H18), C19(H19), C24(H24), C25(H25), C26(H26),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C42(H42),
  C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50),
 C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C30(H30A,H30B,H30C), C32(H32A,H32B,
 H32C)
;
_shelx_res_checksum              94646
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.749
_oxdiff_exptl_absorpt_empirical_full_min 0.665