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_4003509
_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         'C6 F3 I3.57, 1.43(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
_atom_sites_solution_primary     dual
_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                   19.431(11)
_cell_length_b                   13.831(3)
_cell_length_c                   22.900(14)
_cell_measurement_reflns_used    1432
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      17.223
_cell_measurement_theta_min      3.077
_cell_volume                     6154(5)
_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      299.5
_diffrn_measured_fraction_theta_full 0.770
_diffrn_measured_fraction_theta_max 0.770
_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  0.2468
_diffrn_reflns_av_unetI/netI     0.1799
_diffrn_reflns_Laue_measured_fraction_full 0.770
_diffrn_reflns_Laue_measured_fraction_max 0.770
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6141
_diffrn_reflns_point_group_measured_fraction_full 0.770
_diffrn_reflns_point_group_measured_fraction_max 0.770
_diffrn_reflns_theta_full        17.223
_diffrn_reflns_theta_max         17.223
_diffrn_reflns_theta_min         3.077
_exptl_absorpt_coefficient_mu    5.636
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    2.782
_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   20.814
_exptl_transmission_factor_min   3.033
_refine_diff_density_max         3.021
_refine_diff_density_min         -2.706
_refine_diff_density_rms         0.650
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         1432
_refine_ls_number_restraints     802
_refine_ls_restrained_S_all      0.712
_refine_ls_R_factor_all          0.2410
_refine_ls_R_factor_gt           0.1513
_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^)+(0.6000P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3951
_refine_ls_wR_factor_ref         0.5534
_reflns_Friedel_coverage         0.000
_reflns_number_gt                811
_reflns_number_total             1432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            AllHPCIFs.cif
_cod_data_source_block           cotpy_4gpatrans
_cod_database_code               4003509
_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. 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(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C28) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.025
Uanis(C28) \\sim Ueq, Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.005
Uanis(C20) = Uanis(N4) = Uanis(C16) = Uanis(C17) = Uanis(C18) = Uanis(C19)
Uanis(N2) = Uanis(C9) = Uanis(C8) = Uanis(C7)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C18(H18), C17(H17),
 C16(H16), C19(H19), C15(H15), C14(H14), C13(H13), C12(H12), C27(H27), C28(H28),
  C29(H29), C30(H30), C22(H22), C23(H23), C24(H24)
4.b Fitted hexagon refined as free rotating group:
 N1(C1,C2,C3,C4,C5), N2(C6,C7,C8,C9,C10), C18(C17,C16,N4,C20,C19), C35(C36,C31,
 C32,C33,C34), C11(N3,C15,C14,C13,C12), N6(C26,C27,C28,C29,C30), C25(N5,C21,C22,
 C23,C24)
;
_shelx_res_checksum              82058
_shelx_hkl_checksum              7637
_olex2_submission_special_instructions 'No special instructions were received'