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_1566393
_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             2021-08-10
_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                100.301(4)
_cell_angle_beta                 91.468(4)
_cell_angle_gamma                93.516(4)
_cell_formula_units_Z            2
_cell_length_a                   9.8578(5)
_cell_length_b                   10.9457(6)
_cell_length_c                   22.5606(12)
_cell_measurement_reflns_used    5505
_cell_measurement_temperature    130.00(10)
_cell_measurement_theta_max      71.8230
_cell_measurement_theta_min      3.9550
_cell_volume                     2388.9(2)
_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      130.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.970
_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    1.50    --  -41.91 125.00-180.00   90
  2  \w    -92.00  -2.00   1.00    1.50    --  -41.91 125.00 -90.00   90
  3  \w   -108.00 -29.00   1.00    1.50    --  -41.91 -38.00 120.00   79
  4  \w   -115.00 -17.00   1.00    1.50    --  -41.91 -38.00  30.00   98
  5  \w     58.00  98.00   1.00    1.50    --   41.91-125.00   0.00   40
  6  \w     40.00 123.00   1.00    6.00    --  103.72 -61.00   0.00   83
  7  \w     78.00 167.00   1.00    6.00    --  103.72  45.00   0.00   89
  8  \w     78.00 108.00   1.00    6.00    --  103.72 -94.00  30.00   30
  9  \w    140.00 166.00   1.00    6.00    --  103.72  45.00-180.00   26
 10  \w     28.00  77.00   1.00    6.00    --  103.72 -77.00 -30.00   49
 11  \w     27.00 132.00   1.00    6.00    --  103.72 -30.00-180.00  105
 12  \w     92.00 117.00   1.00    6.00    --  103.72-125.00 -30.00   25
 13  \w     41.00 103.00   1.00    6.00    --  103.72-125.00-180.00   62
 14  \w     29.00 136.00   1.00    6.00    --  103.72 -77.00-180.00  107
 15  \w     35.00  62.00   1.00    6.00    --  103.72 -94.00  30.00   27
 16  \w     36.00  63.00   1.00    6.00    --  103.72-125.00-150.00   27
 17  \w     91.00 118.00   1.00    6.00    --  103.72-125.00-150.00   27
 18  \w     84.00 118.00   1.00    6.00    --  103.72-125.00  30.00   34
 19  \w     22.00 155.00   1.00    6.00    --  103.72 -15.00   0.00  133
;
_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      -0.1448020000
_diffrn_orient_matrix_UB_12      0.0198382000
_diffrn_orient_matrix_UB_13      0.0222892000
_diffrn_orient_matrix_UB_21      0.0165385000
_diffrn_orient_matrix_UB_22      -0.0967436000
_diffrn_orient_matrix_UB_23      0.0411208000
_diffrn_orient_matrix_UB_31      0.0575138000
_diffrn_orient_matrix_UB_32      0.1039383000
_diffrn_orient_matrix_UB_33      0.0513410000
_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  0.0494
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17689
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.052
_diffrn_reflns_theta_min         3.986
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.045
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.394
_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    1.575
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.221
_refine_diff_density_max         1.440
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         9136
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0693
_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^)+(0.1178P)^2^+0.3475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1744
_refine_ls_wR_factor_ref         0.1905
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7539
_reflns_number_total             9136
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-100-002y_130_red1_ref
_cod_database_code               1566393
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C46 H38 P2 F12 N14'
_chemical_oxdiff_usercomment     '130 K'
_reflns_odcompleteness_completeness 99.91
_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
 N11A-C23A \\sim N11B-C24B
 with sigma of 0.02
 N11A-C24A \\sim N11B-C23B
 with sigma of 0.02
 N12A-C33A \\sim N12B-C34B
 with sigma of 0.02
 N12A-C34A \\sim N12B-C33B
 with sigma of 0.02
 C27A-C25A \\sim C27B-C26B
 with sigma of 0.02
 C27A-C26A \\sim C27B-C25B
 with sigma of 0.02
 C27A-C28A \\sim C27B-C28B
 with sigma of 0.02
 C23A-C25A \\sim C24B-C26B
 with sigma of 0.02
 C33A-C31A \\sim C34B-C32B
 with sigma of 0.02
 C34A-C32A \\sim C33B-C31B
 with sigma of 0.02
 C32A-C30A \\sim C31B-C30B
 with sigma of 0.02
 C24A-C26A \\sim C23B-C25B
 with sigma of 0.02
 C30A-C31A \\sim C30B-C32B
 with sigma of 0.02
 C30A-C29A \\sim C30B-C29B
 with sigma of 0.02
 C28A-C29A \\sim C28B-C29B
 with sigma of 0.02
 N11A-C25A \\sim N11B-C26B
 with sigma of 0.04
 N11A-C26A \\sim N11B-C25B
 with sigma of 0.04
 N12A-C32A \\sim N12B-C31B
 with sigma of 0.04
 N12A-C31A \\sim N12B-C32B
 with sigma of 0.04
 C27A-C23A \\sim C27B-C24B
 with sigma of 0.04
 C27A-C24A \\sim C27B-C23B
 with sigma of 0.04
 C27A-C29A \\sim C27B-C29B
 with sigma of 0.04
 C23A-C24A \\sim C24B-C23B
 with sigma of 0.04
 C25A-C26A \\sim C26B-C25B
 with sigma of 0.04
 C25A-C28A \\sim C26B-C28B
 with sigma of 0.04
 C33A-C34A \\sim C34B-C33B
 with sigma of 0.04
 C33A-C30A \\sim C34B-C30B
 with sigma of 0.04
 C34A-C30A \\sim C33B-C30B
 with sigma of 0.04
 C32A-C31A \\sim C31B-C32B
 with sigma of 0.04
 C32A-C29A \\sim C31B-C29B
 with sigma of 0.04
 C30A-C28A \\sim C30B-C28B
 with sigma of 0.04
 C26A-C28A \\sim C25B-C28B
 with sigma of 0.04
 C31A-C29A \\sim C32B-C29B
 with sigma of 0.04
 N11B-C23B \\sim N11B-C24B
 with sigma of 0.02
 C33B-C31B \\sim C34B-C32B
 with sigma of 0.02
 C27B-C25B \\sim C27B-C26B
 with sigma of 0.02
 C30B-C32B \\sim C31B-C30B
 with sigma of 0.02
 N12B-C33B \\sim N12B-C34B
 with sigma of 0.02
 C25B-C23B \\sim C26B-C24B
 with sigma of 0.02
3. Restrained planarity
 C26B, C27B, C25B, C23B, N11B, C24B
 with sigma of 0.1
 C27B, C25B, C23B, N11B, C24B, C26B
 with sigma of 0.001
 C34B, N12B, C33B, C31B, C30B, C32B
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C28A) = Uanis(N11A) = Uanis(C23A) = Uanis(C24A) = Uanis(C25A) =
Uanis(C26A) = Uanis(C27A) = Uanis(C29A) = Uanis(C30A) = Uanis(C32A) =
Uanis(C31A) = Uanis(C34A) = Uanis(C33A) = Uanis(N12A) = Uanis(C28B) =
Uanis(C26B) = Uanis(C25B) = Uanis(C27B) = Uanis(C24B) = Uanis(C23B) =
Uanis(C29B) = Uanis(N11B) = Uanis(C30B) = Uanis(C31B) = Uanis(C32B) =
Uanis(C33B) = Uanis(C34B) = Uanis(N12B)
5. Others
 Sof(C29B)=Sof(H29B)=Sof(N11B)=Sof(C24B)=Sof(H24B)=Sof(C23B)=Sof(H23B)=
 Sof(C26B)=Sof(H26B)=Sof(C25B)=Sof(H25B)=Sof(C27B)=Sof(C28B)=Sof(H28B)=
 Sof(C30B)=Sof(C31B)=Sof(H31B)=Sof(C32B)=Sof(H32B)=Sof(C33B)=Sof(H33B)=
 Sof(C34B)=Sof(H34B)=Sof(N12B)=1-FVAR(1)
 Sof(N11A)=Sof(N12A)=Sof(C27A)=Sof(C23A)=Sof(H23A)=Sof(C25A)=Sof(H25A)=
 Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=Sof(C32A)=Sof(H32A)=Sof(C24A)=
 Sof(H24A)=Sof(C30A)=Sof(C26A)=Sof(H26A)=Sof(C31A)=Sof(H31A)=Sof(C28A)=
 Sof(H28A)=Sof(C29A)=Sof(H29A)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 N10(H10), N5(H5), N6(H6), N1(H1), C7(H7), C16(H16), C6(H6a), C2(H2), C22(H22),
  C12(H12), C43(H43), C13(H13), C18(H18), C41(H41), C21(H21), C1(H1a),
 C10(H10a), C40(H40), C5(H5a), C45(H45), C46(H46), C17(H17), C44(H44), C38(H38),
  C36(H36), C37(H37), C23A(H23A), C11(H11), C25A(H25A), C33A(H33A), C34A(H34A),
 C32A(H32A), C24A(H24A), C35(H35), C26A(H26A), C31A(H31A), C28A(H28A),
 C29A(H29A), C29B(H29B), C24B(H24B), C23B(H23B), C26B(H26B), C25B(H25B),
 C28B(H28B), C31B(H31B), C32B(H32B), C33B(H33B), C34B(H34B)
;
_shelx_res_checksum              20026
_shelx_hkl_checksum              82293
_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 1.343
_oxdiff_exptl_absorpt_empirical_full_min 0.731