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_1566402
_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(F6 P), 2(C12 H10 N2)'
_chemical_formula_sum            'C46 H38 F12 Fe N14 P2'
_chemical_formula_weight         1132.69
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_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                79.439(3)
_cell_angle_beta                 89.335(4)
_cell_angle_gamma                89.190(4)
_cell_formula_units_Z            4
_cell_length_a                   9.8294(6)
_cell_length_b                   22.3967(7)
_cell_length_c                   22.3209(10)
_cell_measurement_reflns_used    5812
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      71.9310
_cell_measurement_theta_min      3.9780
_cell_volume                     4829.9(4)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.967
_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   -116.00 -18.00   1.00    3.00    --  -42.16 -38.00  90.00   98
  2  \w   -116.00 -18.00   1.00    3.00    --  -42.16 -38.00-180.00   98
  3  \w   -118.00 -10.00   1.00    3.00    --  -42.16 -77.00 -60.00  108
  4  \w      1.00  70.00   1.00    3.00    --   42.16 -99.00  60.00   69
  5  \w     65.00  94.00   1.00    3.00    --   42.16-125.00 150.00   29
  6  \w     56.00 109.00   1.00   12.00    --  103.72 -94.00 -90.00   53
  7  \w     55.00  96.00   1.00   12.00    --  103.72  15.00-180.00   41
  8  \w     28.00 130.00   1.00   12.00    --  103.72 -30.00-150.00  102
  9  \w     97.00 169.00   1.00   12.00    --  103.72 125.00   0.00   72
 10  \w     53.00  86.00   1.00   12.00    --  103.72 -94.00   0.00   33
 11  \w    132.00 157.00   1.00   12.00    --  103.72 125.00  90.00   25
 12  \w    109.00 178.00   1.00   12.00    --  103.72  15.00-180.00   69
 13  \w     57.00 114.00   1.00   12.00    --  103.72-125.00  90.00   57
 14  \w     42.00 132.00   1.00   12.00    --  103.72 -30.00 -60.00   90
 15  \w     28.00 134.00   1.00   12.00    --  103.72 -77.00  90.00  106
 16  \w     34.00 124.00   1.00   12.00    --  103.72 -30.00  90.00   90
 17  \w     94.00 128.00   1.00   12.00    --  103.72 125.00-150.00   34
 18  \w    101.00 130.00   1.00   12.00    --  103.72-141.00-108.10   29
;
_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      0.1472621238
_diffrn_orient_matrix_UB_12      0.0108380294
_diffrn_orient_matrix_UB_13      -0.0234224838
_diffrn_orient_matrix_UB_21      -0.0172269517
_diffrn_orient_matrix_UB_22      -0.0476113813
_diffrn_orient_matrix_UB_23      -0.0410734600
_diffrn_orient_matrix_UB_31      -0.0508777528
_diffrn_orient_matrix_UB_32      0.0501229416
_diffrn_orient_matrix_UB_33      -0.0519031376
_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  0.0567
_diffrn_reflns_av_unetI/netI     0.0774
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            35116
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.068
_diffrn_reflns_theta_min         4.016
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.002
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.449
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.199
_refine_diff_density_max         1.159
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1432
_refine_ls_number_reflns         18380
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0740
_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^)+(0.0857P)^2^+1.9879P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1818
_refine_ls_wR_factor_ref         0.2099
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11960
_reflns_number_total             18380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-100-002y_160_redup_ref
_cod_database_code               1566402
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C46 H38 P2 F12 N14'
_chemical_oxdiff_usercomment     '160 K'
_reflns_odcompleteness_completeness 99.75
_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 N(H) groups
2. Restrained distances
 P2-F12A \\sim P2-F11B
 with sigma of 0.02
 P2-F10A \\sim P2-F9B
 with sigma of 0.02
 P2-F11A \\sim P2-F10B
 with sigma of 0.02
 P2-F9A \\sim P2-F12B
 with sigma of 0.02
 P1-F6A \\sim P1-F5B
 with sigma of 0.02
 P1-F4A \\sim P1-F3B
 with sigma of 0.02
 P1-F5A \\sim P1-F4B
 with sigma of 0.02
 P1-F3A \\sim P1-F6B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C75A) = Uanis(C75B)
Uanis(C74A) = Uanis(C74B)
4. Rigid body (RIGU) restrains
 P1, F1, F2, F6A, F4A, F5A, F3A, F5B, F3B, F4B, F6B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C75B)=Sof(H75B)=Sof(C74B)=Sof(H74B)=1-FVAR(1)
 Sof(C75A)=Sof(H75A)=Sof(C74A)=Sof(H74A)=FVAR(1)
 Sof(F12B)=Sof(F9B)=Sof(F10B)=Sof(F11B)=1-FVAR(2)
 Sof(F12A)=Sof(F10A)=Sof(F11A)=Sof(F9A)=FVAR(2)
 Sof(F5B)=Sof(F3B)=Sof(F4B)=Sof(F6B)=1-FVAR(3)
 Sof(F6A)=Sof(F4A)=Sof(F5A)=Sof(F3A)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 N5(H5), N1(H1), N16(H16a), N10(H10), N6(H6), N15(H15), N20(H20), N11(H11a),
 C18(H18), C6(H6a), C40(H40), C2(H2), C7(H7), C1(H1a), C38(H38), C39(H39),
 C5(H5a), C13(H13), C27(H27), C34(H34), C21(H21), C48(H48), C35(H35), C90(H90),
 C10(H10a), C16(H16), C17(H17), C32(H32), C12(H12), C43(H43), C23(H23),
 C29(H29), C33(H33), C51(H51), C46(H46), C22(H22), C82(H82), C87(H87), C54(H54),
  C28(H28), C47(H47), C11(H11), C81(H81), C24(H24), C67(H67), C86(H86),
 C68(H68), C69(H69), C50(H50), C65(H65), C84(H84), C55(H55), C66(H66), C89(H89),
  C79(H79), C91(H91), C92(H92), C83(H83), C44(H44), C45(H45), C58(H58),
 C80(H80), C57(H57), C70(H70), C60(H60), C56(H56), C59(H59), C53(H53), C77(H77),
  C78(H78), C63(H63), C62(H62), C71(H71), C72(H72), C75A(H75A), C74A(H74A),
 C75B(H75B), C74B(H74B)
;
_shelx_res_checksum              44356
_shelx_hkl_checksum              52335
_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 2.090
_oxdiff_exptl_absorpt_empirical_full_min 0.661