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_1566397
_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         'C22 H18 Fe N10, 2(C10 H8 N2 S2), 2(F6 P)'
_chemical_formula_sum            'C42 H34 F12 Fe N14 P2 S4'
_chemical_formula_weight         1208.86
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-11
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   14.8052(7)
_cell_length_b                   14.8052(7)
_cell_length_c                   19.695(2)
_cell_measurement_reflns_used    2550
_cell_measurement_temperature    80.1(7)
_cell_measurement_theta_max      65.5890
_cell_measurement_theta_min      4.0960
_cell_volume                     3738.7(5)
_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      80.1(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.973
_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    -65.00  34.00   1.00    4.00    --  -40.41  38.00 -60.00   99
  2  \w     24.00  60.00   1.00    4.00    --   40.41-125.00-180.00   36
  3  \w     47.00  78.00   1.00    4.00    --   40.41-125.00  60.00   31
  4  \w      1.00  34.00   1.00    4.00    --   40.41 -99.00-180.00   33
  5  \w    101.00 132.00   1.00   16.00    --  103.72 125.00-150.00   31
  6  \w    138.00 176.00   1.00   16.00    --  103.72 125.00   0.00   38
  7  \w     34.00 104.00   1.00   16.00    --  103.72 -94.00  30.00   70
  8  \w    103.00 148.00   1.00   16.00    --  103.72 125.00 -30.00   45
  9  \w     53.00 118.00   1.00   16.00    --  103.72 -61.00  60.00   65
;
_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      -0.0022197000
_diffrn_orient_matrix_UB_12      -0.1015112000
_diffrn_orient_matrix_UB_13      0.0203084000
_diffrn_orient_matrix_UB_21      0.1053695000
_diffrn_orient_matrix_UB_22      0.0378402000
_diffrn_orient_matrix_UB_23      -0.0357766000
_diffrn_orient_matrix_UB_31      0.0577218000
_diffrn_orient_matrix_UB_32      0.0519378000
_diffrn_orient_matrix_UB_33      0.0664951000
_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  0.0484
_diffrn_reflns_av_unetI/netI     0.0698
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8959
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.691
_diffrn_reflns_theta_min         4.114
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.443
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.551
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       plate
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.103
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 1261 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.001(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4454
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0609
_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^)+(0.0583P)^2^+3.8705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1481
_refine_ls_wR_factor_ref         0.1571
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                3725
_reflns_number_total             4454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-85-003_hex_80_lattit_ref
_cod_database_code               1566397
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C42 H34 N14 P2 F12 S4'
_chemical_oxdiff_usercomment     '80 K'
_reflns_odcompleteness_completeness 98.34
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.529(3)
 0.471(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
3. Restrained planarity
 F2, F3, P1, F1
 with sigma of 0.001
4. Rigid body (RIGU) restrains
 P2, F7, F4, F5, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P1, F2, F1, F3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C1(H1a), C2(H2), C10(H10), C21(H21), C20(H20), C19(H19), C18(H18),
 C11(H11), C15(H15), C14(H14), C13(H13), C12(H12), N5(H5), C5(H5a), C7(H7),
 C6(H6)
5.b Fitted hexagon refined as free rotating group:
 N7(C21,C20,C19,C18,C17), C16(C15,C14,C13,C12,N6)
;
_shelx_res_checksum              27859
_shelx_hkl_checksum              16950
_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 1.324
_oxdiff_exptl_absorpt_empirical_full_min 0.837