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_4003512
_publ_section_title
;
 Controlling Spin Switching with Anionic Supramolecular Frameworks
;
_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             2019-10-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.208(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2338(4)
_cell_length_b                   12.1188(3)
_cell_length_c                   25.0418(7)
_cell_measurement_reflns_used    8207
_cell_measurement_temperature    173.10(14)
_cell_measurement_theta_max      28.3870
_cell_measurement_theta_min      3.5910
_cell_volume                     5835.7(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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      173.10(14)
_diffrn_detector_area_resol_mean 16.0774
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measurement_details
;
  1 omega  -21.00    4.00   1.0000   15.1300
omega____ theta____ kappa____ phi______ frames
    -       19.6682  -57.0000  -30.0000 25

  2 omega   36.00   64.00   1.0000   15.1300
omega____ theta____ kappa____ phi______ frames
    -       19.6682  -99.0000  -60.0000 28

  3 omega  -93.00    1.00   1.0000   15.1300
omega____ theta____ kappa____ phi______ frames
    -      -22.1682  -57.0000   30.0000 94

  4 omega  -50.00   36.00   1.0000   15.1300
omega____ theta____ kappa____ phi______ frames
    -      -22.1682   77.0000 -180.0000 86

  5 omega  -73.00  -48.00   1.0000   15.1300
omega____ theta____ kappa____ phi______ frames
    -      -22.1682 -179.0000  120.0000 25
;
_diffrn_measurement_device_type  'Oxford Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0328814000
_diffrn_orient_matrix_UB_12      0.0223532000
_diffrn_orient_matrix_UB_13      -0.0064078000
_diffrn_orient_matrix_UB_21      -0.0141217000
_diffrn_orient_matrix_UB_22      0.0539956000
_diffrn_orient_matrix_UB_23      0.0010191000
_diffrn_orient_matrix_UB_31      0.0089582000
_diffrn_orient_matrix_UB_32      0.0032846000
_diffrn_orient_matrix_UB_33      0.0275735000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            25609
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.833
_diffrn_reflns_theta_min         3.165
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.603
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73451
_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    2.259
_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         2.528
_refine_diff_density_min         -2.687
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         13032
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0531P)^2^+47.3591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1294
_refine_ls_wR_factor_ref         0.1370
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10783
_reflns_number_total             13032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Coterpy2_I2_13DITFB_173K_desolvated.cif
_cod_data_source_block           Coterpy2_I2_13DITFB_173K_desolvated
_cod_database_code               4003512
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Co1N6C30I2H22C18I3F3C1O1H4
_reflns_odcompleteness_completeness 85.28
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.77
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C48B \\sim C47B \\sim C46B \\sim F10B \\sim F11B \\sim F12B \\sim C45B \\sim
I6B \\sim C44B \\sim F9B \\sim I5B: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04
F11A \\sim I5A \\sim C43A \\sim C44A \\sim C48A \\sim C45A \\sim F9A \\sim C47A
\\sim F12A \\sim C46A \\sim I6A \\sim F10A \\sim F11B \\sim I5B \\sim C43B
\\sim C44B \\sim C48B \\sim C45B \\sim F9B \\sim C47B \\sim F12B \\sim C46B
\\sim I6B \\sim F10B \\sim C47C \\sim I5C \\sim C43C \\sim C44C \\sim C48C
\\sim C45C \\sim F9C \\sim F12C \\sim I6C \\sim C46C \\sim F11C \\sim F10C:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uiso(I5C) = Uiso(C43C) = Uiso(C44C) = Uiso(C48C) = Uiso(C45C) = Uiso(F9C) =
Uiso(C47C) = Uiso(F12C) = Uiso(I6C) = Uiso(C46C) = Uiso(F11C) = Uiso(F10C)
3. Rigid body (RIGU) restrains
 I5A, I5B, I6A, I6B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: I5A(0.5) C43A(0.5) C44A(0.5) C45A(0.5) C46A(0.5) C47A(0.5)
 C48A(0.5) F9A(0.5) F12A(0.5) F11A(0.5) F10A(0.5) I6A(0.5) I5B(0.35) C43B(0.35)
 C44B(0.35) C45B(0.35) C46B(0.35) C47B(0.35) C48B(0.35) F9B(0.35) F12B(0.35)
 F11B(0.35) F10B(0.35) I6B(0.35) I5C(0.15) C43C(0.15) I6C(0.15) C44C(0.15)
 C45C(0.15) C46C(0.15) C47C(0.15) C48C(0.15) F9C(0.15) F12C(0.15) F11C(0.15)
 F10C(0.15)
5.a Free rotating group:
 I5A(C43A,C44A,C45A,C46A,C47A,C48A,F9A,F12A,F11A,F10A,I6A,I5B,C43B,C44B,C45B,
 C46B,C47B,C48B,F9B,F12B,F11B,F10B,I6B,I5C,C43C,I6C,C44C,C45C,C46C,C47C,C48C,
 F9C,F12C,F11C,F10C)
5.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              47933
_shelx_hkl_checksum              81349
_olex2_submission_special_instructions 'No special instructions were received'