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_1566391
_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 N4), 2(F6 P)'
_chemical_formula_sum            'C42 H34 F12 Fe N18 P2'
_chemical_formula_weight         1136.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-08-10
_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                 98.279(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4569(2)
_cell_length_b                   16.5431(3)
_cell_length_c                   23.9335(4)
_cell_measurement_reflns_used    6540
_cell_measurement_temperature    249.99(11)
_cell_measurement_theta_max      71.7170
_cell_measurement_theta_min      4.2430
_cell_volume                     4880.71(15)
_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      249.99(11)
_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 0.976
_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    -63.00  19.00   1.00    1.00    --  -42.16  57.00 -90.00   82
  2  \w    -70.00  30.00   1.00    1.00    --  -42.16  57.00  30.00  100
  3  \w     34.00  85.00   1.00    1.00    --   42.16-125.00-180.00   51
  4  \w     37.00  84.00   1.00    4.00    --  103.72-125.00   0.00   47
  5  \w     79.00 175.00   1.00    4.00    --  103.72  45.00-180.00   96
  6  \w    133.00 166.00   1.00    4.00    --  103.72 125.00 -60.00   33
  7  \w     71.00 126.00   1.00    4.00    --  103.72  15.00 120.00   55
  8  \w     89.00 165.00   1.00    4.00    --  103.72  45.00 120.00   76
  9  \w     67.00 113.00   1.00    4.00    --  103.72 -30.00 150.00   46
 10  \w     32.00 125.00   1.00    4.00    --  103.72 -61.00  30.00   93
;
_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      -0.0963747000
_diffrn_orient_matrix_UB_12      -0.0355938000
_diffrn_orient_matrix_UB_13      -0.0399929000
_diffrn_orient_matrix_UB_21      0.0038301000
_diffrn_orient_matrix_UB_22      0.0722918000
_diffrn_orient_matrix_UB_23      -0.0402624000
_diffrn_orient_matrix_UB_31      0.0794571000
_diffrn_orient_matrix_UB_32      -0.0466461000
_diffrn_orient_matrix_UB_33      -0.0318254000
_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  0.0295
_diffrn_reflns_av_unetI/netI     0.0358
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20354
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.905
_diffrn_reflns_theta_min         3.733
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.987
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.425
_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    1.547
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         9365
_refine_ls_number_restraints     163
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0913P)^2^+2.9870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1539
_refine_ls_wR_factor_ref         0.1654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7656
_reflns_number_total             9365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-117-002y_250_red_ref
_cod_database_code               1566391
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C42 H34 P2 F12 N18'
_chemical_oxdiff_usercomment     '250 K'
_reflns_odcompleteness_completeness 99.87
_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-F9A \\sim P2-F11A \\sim P2-F8A \\sim P2-F12A
 with sigma of 0.002
 F9A-F11A \\sim F12A-F8A
 with sigma of 0.002
 P2-F10A \\sim P2-F10B
 with sigma of 0.02
 P2-F9A \\sim P2-F8B
 with sigma of 0.02
 P2-F7A \\sim P2-F7B
 with sigma of 0.02
 P2-F12A \\sim P2-F11B
 with sigma of 0.02
 P2-F11A \\sim P2-F9B
 with sigma of 0.02
 P2-F8A \\sim P2-F12B
 with sigma of 0.02
 F11A-F12A \\sim F9A-F8A
 with sigma of 0.002
 F11B-F10B \\sim F7B-F8B
 with sigma of 0.002
 P2-F11B \\sim P2-F10B \\sim P2-F8B \\sim P2-F7B
 with sigma of 0.002
 P2-F9B \\sim P2-F12B
 with sigma of 0.002
 P2-F10A \\sim P2-F7A
 with sigma of 0.02
 P2-F11A \\sim P2-F9A \\sim P2-F8A \\sim P2-F12A
 with sigma of 0.002
3. Restrained planarity
 F11A, F9A, F8A, F12A
 with sigma of 0.001
 F11B, F10B, F7B, F8B
 with sigma of 0.001
 F11B, F7B, F8B, F10B, P2
 with sigma of 0.001
 F11A, F9A, F8A, F12A, P2
 with sigma of 0.001
 F11B, F9B, F8B, F12B, P2
 with sigma of 0.001
4. Rigid body (RIGU) restrains
 P2, F9B, F12B, F8A, F9A, F12A, F11A, F11B, F10B, F7B, F8B, F10A, F7A
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.008
 C38, C39
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.008
5. Others
 Sof(F9B)=Sof(F12B)=Sof(F11B)=Sof(F8B)=Sof(F10B)=Sof(F7B)=1-FVAR(1)
 Sof(F10A)=Sof(F9A)=Sof(F7A)=Sof(F12A)=Sof(F8A)=Sof(F11A)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N10(H10), N6(H6), N5(H5), C5(H5A), C16(H16), C18(H18), C35(H35),
 C7(H7), C2(H2), C1(H1A), C22(H22), C21(H21), C6(H6A), C11(H11), C33(H33),
 C31(H31), C17(H17), C10(H10A), C36(H36), C29(H29), C32(H32), C13(H13),
 C26(H26), C30(H30), C39(H39), C25(H25), C41(H41), C34(H34), C12(H12), C23(H23),
  C24(H24), C42(H42), C40(H40)
;
_shelx_res_checksum              13460
_shelx_hkl_checksum              673
_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 1.121
_oxdiff_exptl_absorpt_empirical_full_min 0.881