Controlling Spin Switching with Anionic Supramolecular Frameworks
Pfrunder, Michael C.; Whittaker, Jacob J.; Parsons, Simon; Moubaraki, Boujemaa; Murray, Keith S.; Moggach, Stephen A.; Sharma, Neeraj; Micallef, Aaron S.; Clegg, Jack K.; McMurtrie, John C.; Chemistry of Materials  (2020) –; doi:10.1021/acs.chemmater.0c00375

data_4003505
_publ_section_title
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 Controlling Spin Switching with Anionic Supramolecular Frameworks
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_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c00375
_journal_year                    2020
_chemical_formula_moiety         'C30 H22 Co N6, 3(C6 F4 I2), 2(I)'
_chemical_formula_sum            'C48 H22 Co F12 I8 N6'
_chemical_formula_weight         1984.84
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-05-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.371(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3934(9)
_cell_length_b                   12.3384(8)
_cell_length_c                   25.1198(13)
_cell_measurement_reflns_used    4415
_cell_measurement_temperature    385(2)
_cell_measurement_theta_max      24.7440
_cell_measurement_theta_min      3.5420
_cell_volume                     6009.0(6)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET)
(compiled Nov 29 2007,17:23:28)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET)
(compiled Nov 29 2007,17:23:28)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET)
(compiled Nov 29 2007,17:23:28)
;
_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    'SIR97 (Altomare, et. al. 1997)'
_diffrn_ambient_temperature      385.15
_diffrn_detector_area_resol_mean 16.0774
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_device_type  'Oxford Gemini'
_diffrn_measurement_method       \w
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            26329
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.874
_diffrn_reflns_theta_min         3.142
_exptl_absorpt_coefficient_mu    4.470
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80214
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3644
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         2.463
_refine_diff_density_min         -4.204
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         13560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1531
_refine_ls_R_factor_gt           0.0934
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1236P)^2^+49.9260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2372
_refine_ls_wR_factor_ref         0.2824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7666
_reflns_number_total             13560
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Coterpy2_I2_13DITFB_385K_desolvated.cif
_cod_data_source_block           Coterpy2_I2_13DITFB_385K_desolvated
_cod_database_code               4003505
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uiso(I5C) = Uiso(C43C) = Uiso(C44C) = Uiso(C48C) = Uiso(C45C) = Uiso(F9C) =
Uiso(C47C) = Uiso(F12C) = Uiso(C46C) = Uiso(I6C) = Uiso(F11C) = Uiso(F10C)
3. Others
 Fixed Sof: I5A(0.5) C43A(0.5) C44A(0.5) C45A(0.5) C48A(0.5) C47A(0.5)
 C46A(0.5) F9A(0.5) F12A(0.5) F11A(0.5) F10A(0.5) I6A(0.5) I5B(0.25) C43B(0.25)
 C44B(0.25) C45B(0.25) C48B(0.25) C47B(0.25) C46B(0.25) F9B(0.25) F12B(0.25)
 F11B(0.25) F10B(0.25) I6B(0.25) I5C(0.25) C43C(0.25) C44C(0.25) C45C(0.25)
 C48C(0.25) C47C(0.25) C46C(0.25) F9C(0.25) F12C(0.25) F11C(0.25) F10C(0.25)
 I6C(0.25)
4.a Free rotating group:
 I5A(C43A,C44A,C45A,C48A,C47A,C46A,F9A,F12A,F11A,F10A,I6A), I5B(C43B,C44B,C45B,
 C48B,C47B,C46B,F9B,F12B,F11B,F10B,I6B), I5C(C43C,C44C,C45C,C48C,C47C,C46C,F9C,
 F12C,F11C,F10C,I6C)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C30(H30), C29(H29), C28(H28), C27(H27), C24(H24), C23(H23),
  C22(H22), C19(H19), C18(H18), C17(H17), C16(H16)
;
_shelx_res_checksum              17345
_shelx_hkl_checksum              87176
_olex2_submission_special_instructions 'No special instructions were received'