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_4003514
_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, C6 F3 I3, 2(I)'
_chemical_formula_sum            'C36 H22 Co F3 I5 N6'
_chemical_formula_weight         1289.02
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-05-17
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.3703(3)
_cell_length_b                   15.2991(2)
_cell_length_c                   24.2579(3)
_cell_measurement_reflns_used    32080
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.8640
_cell_measurement_theta_min      3.2104
_cell_volume                     7559.91(18)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_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(2)
_diffrn_detector_area_resol_mean 16.0774
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_details
;
  1 omega   58.00   92.00   1.0000    7.2800
omega____ theta____ kappa____ phi______ frames
    -       20.2984  179.0000 -150.0000 34

  2 omega  -26.00   22.00   1.0000    7.2800
omega____ theta____ kappa____ phi______ frames
    -       20.2984   99.0000 -100.0000 48

  3 omega  -10.00   25.00   1.0000    7.2800
omega____ theta____ kappa____ phi______ frames
    -       20.2984    0.0000   90.0000 35

  4 omega   60.00   86.00   1.0000    7.2800
omega____ theta____ kappa____ phi______ frames
    -       20.2984    0.0000   90.0000 26

  5 omega  -48.00   49.00   1.0000    7.2800
omega____ theta____ kappa____ phi______ frames
    -      -21.8609   77.0000   30.0000 97

  6 omega -102.00  -73.00   1.0000    7.2800
omega____ theta____ kappa____ phi______ frames
    -      -21.8609  179.0000   30.0000 29

  7 omega  -97.00    7.00   1.0000    7.2800
omega____ theta____ kappa____ phi______ frames
    -      -21.8609  -37.0000 -120.0000 104

  8 omega  -44.00  -18.00   1.0000    7.2800
omega____ theta____ kappa____ phi______ frames
    -      -21.8609   77.0000 -180.0000 26

  9 omega  -10.00   32.00   1.0000    7.2800
omega____ theta____ kappa____ phi______ frames
    -      -21.8609   77.0000 -180.0000 42

 10 omega  -62.00  -32.00   1.0000    7.2800
omega____ theta____ kappa____ phi______ frames
    -      -21.8609  179.0000   30.0000 30
;
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0137465000
_diffrn_orient_matrix_UB_12      0.0161526000
_diffrn_orient_matrix_UB_13      -0.0248653000
_diffrn_orient_matrix_UB_21      -0.0316048000
_diffrn_orient_matrix_UB_22      0.0001960000
_diffrn_orient_matrix_UB_23      -0.0122647000
_diffrn_orient_matrix_UB_31      -0.0049644000
_diffrn_orient_matrix_UB_32      0.0434547000
_diffrn_orient_matrix_UB_33      0.0092940000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            60899
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.927
_diffrn_reflns_theta_min         3.304
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.588
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4792
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.104
_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     460
_refine_ls_number_reflns         9263
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0235
_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^)+(0.0227P)^2^+3.8767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0462
_refine_ls_wR_factor_ref         0.0479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7565
_reflns_number_total             9263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Coterpy2_I2_135TITFB_173K.cif
_cod_data_source_block           Coterpy2_I2_135TITFB_173K
_cod_database_code               4003514
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Co1N6C30H22I2C6I3F3
_chemical_oxdiff_usercomment     '[Co(terpy)2]I2 1,3,5 crystal 3'
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C3(H3), C2(H2), C1(H1), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13),
 C14(H14), C15(H15), C19(H19), C18(H18), C17(H17), C16(H16), C22(H22), C23(H23),
  C24(H24), C27(H27), C28(H28), C29(H29), C30(H30)
;
_shelx_res_checksum              61036
_shelx_hkl_checksum              93934
_olex2_submission_special_instructions 'No special instructions were received'