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_1566400
_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 H12 N2)'
_chemical_formula_sum            'C46 H42 F12 Fe N14 P2'
_chemical_formula_weight         1136.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                 101.5451(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.45496(9)
_cell_length_b                   17.98580(15)
_cell_length_c                   14.95322(14)
_cell_measurement_reflns_used    16397
_cell_measurement_temperature    80.0(5)
_cell_measurement_theta_max      71.8540
_cell_measurement_theta_min      3.8540
_cell_volume                     2491.42(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      80.0(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_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 -11.00   1.00    1.00    --  -42.16 125.00-120.00   52
  2  \w   -116.00 -18.00   1.00    1.00    --  -42.16 -38.00   0.00   98
  3  \w   -105.00 -18.00   1.00    1.00    --  -42.16 -38.00  90.00   87
  4  \w     25.00  83.00   1.00    1.00    --   42.16 -99.00  60.00   58
  5  \w      6.00  31.00   1.00    1.00    --   42.16  88.00 172.59   25
  6  \w    -36.00  24.00   1.00    1.00    --   42.16   0.00  30.00   60
  7  \w     76.00 101.00   1.00    4.00    --  103.72  61.00 120.00   25
  8  \w     75.00 178.00   1.00    4.00    --  103.72  30.00 -90.00  103
  9  \w     80.00 175.00   1.00    4.00    --  103.72  45.00-180.00   95
 10  \w     22.00 106.00   1.00    4.00    --  103.72 -94.00  90.00   84
 11  \w     78.00 105.00   1.00    4.00    --  103.72  45.00 150.00   27
 12  \w     81.00 170.00   1.00    4.00    --  103.72  30.00 -30.00   89
 13  \w     71.00  97.00   1.00    4.00    --  103.72  77.00  60.00   26
 14  \w     85.00 115.00   1.00    4.00    --  103.72  61.00  60.00   30
 15  \w     72.00  97.00   1.00    4.00    --  103.72  77.00  90.00   25
 16  \w    116.00 175.00   1.00    4.00    --  103.72  77.00 120.00   59
 17  \w     67.00 121.00   1.00    4.00    --  103.72 -30.00  90.00   54
 18  \w    105.00 176.00   1.00    4.00    --  103.72  77.00  90.00   71
 19  \w     31.00  65.00   1.00    4.00    --  103.72 -30.00  90.00   34
 20  \w    117.00 174.00   1.00    4.00    --  103.72  77.00  60.00   57
 21  \w     76.00 103.00   1.00    4.00    --  103.72  61.00 150.00   27
 22  \w    151.00 176.00   1.00    4.00    --  103.72  61.00 150.00   25
 23  \w     72.00  97.00   1.00    4.00    --  103.72  77.00 120.00   25
 24  \w     75.00 102.00   1.00    4.00    --  103.72 -94.00-180.00   27
 25  \w     76.00 110.00   1.00    4.00    --  103.72  61.00  90.00   34
 26  \w     81.00 108.00   1.00    4.00    --  103.72  45.00 120.00   27
 27  \w     72.00  99.00   1.00    4.00    --  103.72  73.00  80.28   27
;
_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      0.1536403000
_diffrn_orient_matrix_UB_12      -0.0282874000
_diffrn_orient_matrix_UB_13      -0.0005826000
_diffrn_orient_matrix_UB_21      -0.0015864000
_diffrn_orient_matrix_UB_22      0.0417327000
_diffrn_orient_matrix_UB_23      -0.0901533000
_diffrn_orient_matrix_UB_31      0.0636490000
_diffrn_orient_matrix_UB_32      0.0692382000
_diffrn_orient_matrix_UB_33      0.0541202000
_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  0.0278
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21379
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.962
_diffrn_reflns_theta_min         3.892
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.879
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.229
_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    1.515
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.378
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.011(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         9538
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0649P)^2^+0.5030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0923
_reflns_Friedel_coverage         0.936
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                9425
_reflns_number_total             9538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-103-002_t80_red_ref
_cod_database_code               1566400
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C42 H38 P2 F12 N14'
_chemical_oxdiff_usercomment     '80 K Flash Frozen'
_shelx_estimated_absorpt_t_max   0.511
_shelx_estimated_absorpt_t_min   0.322
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.989(3)
 0.011(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(F6A) = Uanis(F6B)
Uanis(F3A) = Uanis(F3B)
Uanis(F4A) = Uanis(F4B)
Uanis(F5A) = Uanis(F5B)
4. Rigid body (RIGU) restrains
 P1, F4B, F3B, F5B, F6B, F6A, F3A, F4A, F1, F5A, F2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F6B)=Sof(F3B)=Sof(F4B)=Sof(F5B)=1-FVAR(1)
 Sof(F3A)=Sof(F6A)=Sof(F4A)=Sof(F5A)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C40(H40A,H40B), C29(H29A,H29B), C28(H28A,H28B)
6.b Aromatic/amide H refined with riding coordinates:
 N10(H10), N5(H5), N6(H6), N1(H1), C22(H22), C21(H21), C11(H11), C10(H10A),
 C43(H43), C17(H17), C32(H32), C16(H16), C37(H37), C18(H18), C7(H7), C46(H46),
 C5(H5A), C6(H6A), C44(H44), C13(H13), C33(H33), C26(H26), C23(H23), C24(H24),
 C12(H12), C35(H35), C25(H25), C36(H36), C2(H2), C31(H31), C45(H45), C34(H34),
 C38(H38), C1(H1A)
;
_shelx_res_checksum              35623
_shelx_hkl_checksum              11372
_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 1.212
_oxdiff_exptl_absorpt_empirical_full_min 0.830