Co-crystallisation as a Modular Approach to the Discovery of Spin-Crossover Materials
Birchall, Lee; Truccolo, Giada; Jackson, Lewis; Shepherd, Helena Jane; Chemical Science  (2022) –; doi:10.1039/D1SC04956A

data_1566390
_publ_section_title
;
 Co-crystallisation as a Modular Approach to the Discovery of
 Spin-Crossover Materials
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC04956A
_journal_year                    2022
_chemical_formula_moiety         '2(C11 H9 Fe0.5 N5), 2(B F4), C2 H6 O'
_chemical_formula_sum            'C24 H24 B2 F8 Fe N10 O'
_chemical_formula_weight         698.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-11 deposited with the CCDC.	2022-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.2860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.4712(2)
_cell_length_b                   17.30860(10)
_cell_length_c                   18.6657(2)
_cell_measurement_reflns_used    10481
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.8190
_cell_measurement_theta_min      3.7010
_cell_volume                     6075.04(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2013/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -92.00  -2.00   1.00    3.00    --  -42.16 125.00 150.00   90
  2  \w   -115.00 -14.00   1.00    3.00    --  -42.16 -57.00 150.00  101
  3  \w   -116.00 -18.00   1.00    3.00    --  -42.16 -38.00-120.00   98
  4  \w     21.00 109.00   1.00   12.00    --  103.72 -94.00 -30.00   88
  5  \w     78.00 177.00   1.00   12.00    --  103.72  45.00-150.00   99
  6  \w     28.00 136.00   1.00   12.00    --  103.72 -77.00 120.00  108
  7  \w     31.00 130.00   1.00   12.00    --  103.72 -45.00  90.00   99
  8  \w     75.00 178.00   1.00   12.00    --  103.72  30.00 -90.00  103
  9  \w     31.00 133.00   1.00   12.00    --  103.72 -61.00-120.00  102
 10  \w   -115.00 -76.00   1.00    3.00    --  -42.16 -57.00  30.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0163434000
_diffrn_orient_matrix_UB_12      0.0202499000
_diffrn_orient_matrix_UB_13      0.0857264000
_diffrn_orient_matrix_UB_21      0.0789189000
_diffrn_orient_matrix_UB_22      -0.0201570000
_diffrn_orient_matrix_UB_23      0.0219858000
_diffrn_orient_matrix_UB_31      0.0149286000
_diffrn_orient_matrix_UB_32      0.0842750000
_diffrn_orient_matrix_UB_33      -0.0153231000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0188
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17359
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.970
_diffrn_reflns_theta_min         3.471
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.777
_exptl_absorpt_correction_T_max  0.53621
_exptl_absorpt_correction_T_min  0.49768
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       block
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.146
_exptl_crystal_size_rad          0.099
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         5876
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0477P)^2^+4.9266P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5544
_reflns_number_total             5876
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-07-006-full-redprac-refprac
_cod_original_cell_volume        6075.04(10)
_cod_database_code               1566390
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C26 H24 N10 B2 F8 O'
_chemical_oxdiff_usercomment     'EtOH/Tol vap diffl 150 K'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 F8A-F6A \\sim F5B-F8B
 with sigma of 0.04
 F7A-B2A \\sim F7B-B2B
 with sigma of 0.02
 F8A-B2A \\sim F5B-B2B
 with sigma of 0.02
 B2A-F5A \\sim B2B-F6B
 with sigma of 0.02
 B2A-F6A \\sim B2B-F8B
 with sigma of 0.02
 F8A-F5A \\sim F5B-F6B
 with sigma of 0.04
 F5A-F6A \\sim F6B-F8B
 with sigma of 0.04
 F7A-F8A \\sim F7B-F5B
 with sigma of 0.04
 F7A-F5A \\sim F7B-F6B
 with sigma of 0.04
 F7A-F6A \\sim F7B-F8B
 with sigma of 0.04
 B2B-F7B \\sim B2B-F5B \\sim B2B-F6B \\sim B2B-F8B
 with sigma of 0.02
 F7A-F8A \\sim F7A-F5A \\sim F7A-F6A \\sim F8A-F5A \\sim F8A-F6A \\sim F5A-F6A
 with sigma of 0.04
 B2A-F7A \\sim B2A-F8A \\sim B2A-F5A \\sim B2A-F6A
 with sigma of 0.02
 F7B-F5B \\sim F7B-F8B \\sim F5B-F8B \\sim F6B-F8B
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 B2B, F7B, F5B, F6B, F8B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B2A, F7A, F8A, F5A, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(B2B)=Sof(F7B)=Sof(F5B)=Sof(F6B)=Sof(F8B)=1-FVAR(1)
 Sof(F7A)=Sof(F8A)=Sof(B2A)=Sof(F5A)=Sof(F6A)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B)
5.b Aromatic/amide H refined with riding coordinates:
 N10(H10), N5(H5), N6(H6), N1(H1), C21(H21), C22(H22), C18(H18), C12(H12),
 C16(H16), C2(H2), C10(H10A), C13(H13), C1(H1A), C11(H11), C5(H5A), C7(H7),
 C17(H17), C6(H6A)
5.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C)
5.d Idealised tetrahedral OH refined as rotating group:
 O1(H1B)
;
_shelx_res_checksum              37592
_shelx_hkl_checksum              95706
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.231
_oxdiff_exptl_absorpt_empirical_full_min 0.853