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_1566382
_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(C10 H8 N4)'
_chemical_formula_sum            'C42 H34 F12 Fe N18 P2'
_chemical_formula_weight         1136.66
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-08
_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                102.939(3)
_cell_angle_beta                 90.267(3)
_cell_angle_gamma                90.662(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9994(4)
_cell_length_b                   11.0389(4)
_cell_length_c                   22.5035(9)
_cell_measurement_reflns_used    6055
_cell_measurement_temperature    264.98(18)
_cell_measurement_theta_max      71.4790
_cell_measurement_theta_min      4.0030
_cell_volume                     2420.69(17)
_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      264.98(18)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.949
_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 -23.00   1.00    1.50    --  -42.16 -38.00 -90.00   93
  2  \w   -118.00 -17.00   1.00    1.50    --  -42.16 -77.00  30.00  101
  3  \w      2.00  83.00   1.00    1.50    --   42.16 -99.00 150.00   81
  4  \w    108.00 177.00   1.00    6.00    --  103.72 125.00 -90.00   69
  5  \w     33.00 109.00   1.00    6.00    --  103.72 -94.00-150.00   76
  6  \w     37.00 125.00   1.00    6.00    --  103.72 -30.00 -60.00   88
  7  \w     68.00 125.00   1.00    6.00    --  103.72  15.00 150.00   57
  8  \w     44.00 117.00   1.00    6.00    --  103.72-125.00 150.00   73
  9  \w     31.00 133.00   1.00    6.00    --  103.72 -77.00 -60.00  102
 10  \w     80.00 175.00   1.00    6.00    --  103.72  45.00 -30.00   95
 11  \w     41.00 131.00   1.00    6.00    --  103.72 -30.00 150.00   90
;
_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      0.0566418000
_diffrn_orient_matrix_UB_12      -0.0122893000
_diffrn_orient_matrix_UB_13      -0.0645952000
_diffrn_orient_matrix_UB_21      0.1137181000
_diffrn_orient_matrix_UB_22      0.0921429000
_diffrn_orient_matrix_UB_23      0.0261772000
_diffrn_orient_matrix_UB_31      0.0871811000
_diffrn_orient_matrix_UB_32      -0.1089336000
_diffrn_orient_matrix_UB_33      0.0087456000
_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  0.0220
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14363
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.000
_diffrn_reflns_theta_min         4.031
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.019
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.402
_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    1.559
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.563
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.051
_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     657
_refine_ls_number_reflns         9056
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0529
_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^)+(0.0834P)^2^+0.9399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1439
_refine_ls_wR_factor_ref         0.1516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7861
_reflns_number_total             9056
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-117-002r_c265_red_ref
_cod_database_code               1566382
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C42 H34 N18 P2 F12'
_chemical_oxdiff_usercomment     '265 K'
_reflns_odcompleteness_completeness 98.67
_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
 N14A-C31A \\sim N14B-C32B
 with sigma of 0.02
 N14A-C32A \\sim N14B-C31B
 with sigma of 0.02
 N11A-C24A \\sim N11B-C23B
 with sigma of 0.02
 N11A-C23A \\sim N11B-C24B
 with sigma of 0.02
 C28A-C29A \\sim C28B-C30B
 with sigma of 0.02
 C28A-C30A \\sim C28B-C29B
 with sigma of 0.02
 C31A-C29A \\sim C32B-C30B
 with sigma of 0.02
 C25A-C23A \\sim C26B-C24B
 with sigma of 0.02
 C25A-C27A \\sim C26B-C27B
 with sigma of 0.02
 C30A-C32A \\sim C29B-C31B
 with sigma of 0.02
 C24A-C26A \\sim C23B-C25B
 with sigma of 0.02
 C27A-C26A \\sim C27B-C25B
 with sigma of 0.02
 N14A-C29A \\sim N14B-C30B
 with sigma of 0.04
 N14A-C30A \\sim N14B-C29B
 with sigma of 0.04
 N11A-C25A \\sim N11B-C26B
 with sigma of 0.04
 N11A-C26A \\sim N11B-C25B
 with sigma of 0.04
 C28A-N13A \\sim C28B-N13B
 with sigma of 0.04
 C28A-C31A \\sim C28B-C32B
 with sigma of 0.04
 C28A-C27A \\sim C28B-C27B
 with sigma of 0.04
 C28A-C32A \\sim C28B-C31B
 with sigma of 0.04
 C28A-N12A \\sim C28B-N12B
 with sigma of 0.04
 N13A-C29A \\sim N13B-C30B
 with sigma of 0.04
 N13A-C25A \\sim N13B-C26B
 with sigma of 0.04
 N13A-C30A \\sim N13B-C29B
 with sigma of 0.04
 N13A-C27A \\sim N13B-C27B
 with sigma of 0.04
 N13A-C26A \\sim N13B-C25B
 with sigma of 0.04
 N13A-N12A \\sim N13B-N12B
 with sigma of 0.04
 C31A-C32A \\sim C32B-C31B
 with sigma of 0.04
 C29A-C30A \\sim C30B-C29B
 with sigma of 0.04
 C29A-N12A \\sim C30B-N12B
 with sigma of 0.04
 C25A-C26A \\sim C26B-C25B
 with sigma of 0.04
 C25A-N12A \\sim C26B-N12B
 with sigma of 0.04
 C30A-N12A \\sim C29B-N12B
 with sigma of 0.04
 C24A-C23A \\sim C23B-C24B
 with sigma of 0.04
 C24A-C27A \\sim C23B-C27B
 with sigma of 0.04
 C23A-C27A \\sim C24B-C27B
 with sigma of 0.04
 C27A-N12A \\sim C27B-N12B
 with sigma of 0.04
 C26A-N12A \\sim C25B-N12B
 with sigma of 0.04
 P1A-F2A \\sim P1A-F6A \\sim P1A-F5A \\sim P1A-F3A
 with sigma of 0.02
 P1A-F1A \\sim P1A-F4A
 with sigma of 0.02
 P1A-F6A \\sim P1B-F5B
 with sigma of 0.02
 P1A-F1A \\sim P1B-F1B
 with sigma of 0.02
 P1A-F3A \\sim P1B-F2B
 with sigma of 0.02
 P1A-F4A \\sim P1B-F4B
 with sigma of 0.02
 P1A-F2A \\sim P1B-F6B
 with sigma of 0.02
 P1A-F5A \\sim P1B-F3B
 with sigma of 0.02
 F6A-F1A \\sim F5B-F1B
 with sigma of 0.04
 F6A-F3A \\sim F5B-F2B
 with sigma of 0.04
 F6A-F4A \\sim F5B-F4B
 with sigma of 0.04
 F6A-F2A \\sim F5B-F6B
 with sigma of 0.04
 F6A-F5A \\sim F5B-F3B
 with sigma of 0.04
 F1A-F3A \\sim F1B-F2B
 with sigma of 0.04
 F1A-F4A \\sim F1B-F4B
 with sigma of 0.04
 F1A-F2A \\sim F1B-F6B
 with sigma of 0.04
 F1A-F5A \\sim F1B-F3B
 with sigma of 0.04
 F3A-F4A \\sim F2B-F4B
 with sigma of 0.04
 F3A-F2A \\sim F2B-F6B
 with sigma of 0.04
 F3A-F5A \\sim F2B-F3B
 with sigma of 0.04
 F4A-F2A \\sim F4B-F6B
 with sigma of 0.04
 F4A-F5A \\sim F4B-F3B
 with sigma of 0.04
 F2A-F5A \\sim F6B-F3B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(N12B) = Uanis(N13B) = Uanis(C27B) = Uanis(C28B) = Uanis(C26B) =
Uanis(C25B) = Uanis(C30B) = Uanis(C29B) = Uanis(C24B) = Uanis(C23B) =
Uanis(C32B) = Uanis(C31B) = Uanis(N11B) = Uanis(N14B) = Uanis(N13A) =
Uanis(N14A) = Uanis(C31A) = Uanis(C32A) = Uanis(C29A) = Uanis(C30A) =
Uanis(C28A) = Uanis(N12A) = Uanis(C27A) = Uanis(C25A) = Uanis(C26A) =
Uanis(C23A) = Uanis(C24A) = Uanis(N11A)
4. Others
 Sof(N12B)=Sof(C28B)=Sof(C30B)=Sof(H30B)=Sof(C32B)=Sof(H32B)=Sof(N14B)=
 Sof(C31B)=Sof(H31B)=Sof(C29B)=Sof(H29B)=Sof(N13B)=Sof(C27B)=Sof(C25B)=
 Sof(H25B)=Sof(C23B)=Sof(H23B)=Sof(N11B)=Sof(C24B)=Sof(H24B)=Sof(C26B)=
 Sof(H26B)=1-FVAR(1)
 Sof(C28A)=Sof(C30A)=Sof(H30A)=Sof(C32A)=Sof(H32A)=Sof(N14A)=Sof(C31A)=
 Sof(H31A)=Sof(C29A)=Sof(H29A)=Sof(N13A)=Sof(C27A)=Sof(C25A)=Sof(H25A)=
 Sof(C23A)=Sof(H23A)=Sof(N11A)=Sof(C24A)=Sof(H24A)=Sof(C26A)=Sof(H26A)=
 Sof(N12A)=FVAR(1)
 Sof(F3B)=Sof(P1B)=Sof(F4B)=Sof(F2B)=Sof(F5B)=Sof(F1B)=Sof(F6B)=1-FVAR(2)
 Sof(P1A)=Sof(F6A)=Sof(F1A)=Sof(F3A)=Sof(F4A)=Sof(F2A)=Sof(F5A)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 N5(H5), N1(H1), N10(H10), N6(H6), C7(H7), C5(H5A), C18(H18), C13(H13),
 C6(H6A), C16(H16), C17(H17), C39(H39), C40(H40), C35(H35), C42(H42), C10(H10A),
  C12(H12), C21(H21), C41(H41), C2(H2), C34(H34), C11(H11), C33(H33), C36(H36),
 C22(H22), C1(H1A), C30A(H30A), C32A(H32A), C31A(H31A), C29A(H29A), C25A(H25A),
 C23A(H23A), C24A(H24A), C26A(H26A), C30B(H30B), C32B(H32B), C31B(H31B),
 C29B(H29B), C25B(H25B), C23B(H23B), C24B(H24B), C26B(H26B)
5.b Fitted hexagon refined as free rotating group:
 C28A(C30A,C32A,N14A,C31A,C29A), C27A(C25A,C23A,N11A,C24A,C26A), C28B(C30B,
 C32B,N14B,C31B,C29B), C27B(C25B,C23B,N11B,C24B,C26B)
;
_shelx_res_checksum              91844
_shelx_hkl_checksum              92203
_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 1.149
_oxdiff_exptl_absorpt_empirical_full_min 0.831