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_7700426
_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         'C34 H48 Fe N4 O2, 2(C H4 O), C24 H20 B'
_chemical_formula_sum            'C60 H76 B Fe N4 O4'
_chemical_formula_weight         983.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-09-04
_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                90
_cell_angle_beta                 114.96(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.520(4)
_cell_length_b                   13.190(3)
_cell_length_c                   22.390(5)
_cell_measurement_reflns_used    4547
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.032
_cell_measurement_theta_min      0.407
_cell_volume                     5494(2)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            201292
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.894
_diffrn_reflns_theta_min         1.130
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.323
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
XDS was used for absorption correction. 
No further details are reported by XDS.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       plate
_exptl_crystal_F_000             2108
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, methanol'
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.011
_exptl_transmission_factor_max   'not given by XDS'
_exptl_transmission_factor_min   'not given by XDS'
_refine_diff_density_max         1.188
_refine_diff_density_min         -1.098
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     660
_refine_ls_number_reflns         16183
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0688
_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^)+(0.1218P)^2^+3.1313P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2010
_refine_ls_wR_factor_ref         0.2124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13079
_reflns_number_total             16183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02372k3.cif
_cod_data_source_block           4-fe
_cod_depositor_comments
'Adding full bibliography for 7700424--7700427.cif.'
_cod_database_code               7700426
_shelx_shelxl_version_number     2016/6
_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, All O(H) groups
2. Restrained distances
 C11-C12 = C11-C13 = C11-C14 = C11-C12A = C11-C13A = C11-C14A
 1.53588 with sigma of 0.001
 C12-C13 = C13-C14 = C14-C12 = C12A-C13A = C13A-C14A = C14A-C12A
 2.49113 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C12) = Uanis(C12A)
Uanis(C13) = Uanis(C13A)
Uanis(C14) = Uanis(C14A)
4. Others
 Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C13A)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(1)
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C29(H29), C32(H32)
5.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C21(H21A,H21B), C22(H22A,H22B), C28(H28A,H28B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C17(H17), C18(H18), C19(H19), C24(H24), C25(H25), C26(H26),
 C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52),
 C54(H54), C55(H55), C56(H56), C57(H57), C58(H58)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C30(H30A,H30B,H30C),
 C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C12A(H12D,H12E,H12F),
 C13A(H13D,H13E,H13F), C14A(H14D,H14E,H14F), C59(H59A,H59B,H59C), C60(H60A,H60B,
 H60C)
5.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4A)
;
_shelx_res_checksum              47172
_olex2_submission_special_instructions 'No special instructions were received'