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_4003506
_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         'C6 F3 I3, 2(I), C30 H22 Co N6'
_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
_audit_creation_date             2019-11-08
_audit_creation_method
;
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                   20.314(3)
_cell_length_b                   15.0560(14)
_cell_length_c                   24.098(3)
_cell_measurement_reflns_used    1597
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.812
_cell_measurement_theta_min      3.406
_cell_volume                     7370.3(16)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.414
_diffrn_measured_fraction_theta_max 0.414
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1261
_diffrn_reflns_av_unetI/netI     0.1097
_diffrn_reflns_Laue_measured_fraction_full 0.414
_diffrn_reflns_Laue_measured_fraction_max 0.414
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6923
_diffrn_reflns_point_group_measured_fraction_full 0.414
_diffrn_reflns_point_group_measured_fraction_max 0.414
_diffrn_reflns_theta_full        20.812
_diffrn_reflns_theta_max         20.812
_diffrn_reflns_theta_min         3.406
_exptl_absorpt_coefficient_mu    4.706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             4792
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.625
_exptl_transmission_factor_min   0.386
_refine_diff_density_max         0.957
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         1597
_refine_ls_number_restraints     497
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_gt           0.0737
_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^)+(0.1481P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1817
_refine_ls_wR_factor_ref         0.2101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1077
_reflns_number_total             1597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            AllHPCIFs.cif
_cod_data_source_block           cotpy_1gpa
_cod_original_cell_volume        7370.3(18)
_cod_database_code               4003506
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details   'CrysAlis, (Oxford Diffraction, 2002)'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C11-C10
 1.493 with sigma of 0.02
 Co1-N1
 2.1 with sigma of 0.02
 Co1-N3
 2.1 with sigma of 0.02
 C21-C20 = C26-C25
 1.493 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(F3) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F1) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.0025
Uanis(Co1) \\sim Ueq: with sigma of 0.0005 and sigma for terminal atoms of
0.00025
Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq,
Uanis(C4) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.0025
Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.0025
Uanis(C35) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.0025
Uanis(C20) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.0025
Uanis(C25) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.0025
Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(N1) \\sim
Ueq, Uanis(N6) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.005 and sigma
for terminal atoms of 0.0025
Uanis(C20) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C30) \\sim Ueq:
with sigma of 0.05 and sigma for terminal atoms of 0.025
4.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14), C15(H15), C24(H24),
 C23(H23), C22(H22), C1(H1), C2(H2), C3(H3), C4(H4), C29(H29), C28(H28),
 C27(H27), C30(H30), C17(H17), C16(H16), C19(H19), C18(H18)
4.b Fitted hexagon refined as free rotating group:
 N2(C6,C7,C8,C9,C10), C11(C12,C13,C14,C15,N3), N5(C25,C24,C23,C22,C21),
 C31(C32,C33,C34,C35,C36), N1(C1,C2,C3,C4,C5), C29(C28,C27,C26,N6,C30), C17(C16,
 N4,C20,C19,C18)
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_shelx_res_checksum              82261
_shelx_hkl_checksum              85827
_olex2_submission_special_instructions 'No special instructions were received'