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_1566398
_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
_atom_sites_solution_primary     dual
_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                97.221(2)
_cell_angle_beta                 96.811(2)
_cell_angle_gamma                93.568(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2078(2)
_cell_length_b                   11.4083(2)
_cell_length_c                   21.4035(4)
_cell_measurement_reflns_used    15994
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      71.7840
_cell_measurement_theta_min      3.8860
_cell_volume                     2447.76(8)
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(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 0.973
_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    -67.00  32.00   1.00    2.00    --  -42.16  38.00 -60.00   99
  2  \w   -116.00 -18.00   1.00    2.00    --  -42.16 -38.00 120.00   98
  3  \w    -70.00  31.00   1.00    2.00    --  -42.16  57.00  60.00  101
  4  \w     23.00  98.00   1.00    2.00    --   42.16-125.00 120.00   75
  5  \w     23.00  98.00   1.00    2.00    --   42.16-125.00 -90.00   75
  6  \w     31.00 133.00   1.00    8.00    --  103.72 -61.00 -90.00  102
  7  \w     27.00 132.00   1.00    8.00    --  103.72 -30.00 150.00  105
  8  \w     28.00 136.00   1.00    8.00    --  103.72 -77.00  90.00  108
  9  \w     21.00 109.00   1.00    8.00    --  103.72 -94.00-180.00   88
 10  \w     75.00 178.00   1.00    8.00    --  103.72  30.00-180.00  103
 11  \w     78.00 177.00   1.00    8.00    --  103.72  45.00 -30.00   99
 12  \w     31.00 118.00   1.00    8.00    --  103.72-125.00 150.00   87
 13  \w     31.00 118.00   1.00    8.00    --  103.72-125.00  90.00   87
 14  \w     21.00 109.00   1.00    8.00    --  103.72 -94.00 -90.00   88
 15  \w     94.00 177.00   1.00    8.00    --  103.72 125.00 120.00   83
 16  \w     22.00 156.00   1.00    8.00    --  103.72 -15.00   0.00  134
 17  \w   -115.00 -14.00   1.00    2.00    --  -42.16 -57.00  30.00  101
 18  \w   -118.00 -39.00   1.00    2.00    --  -42.16 -77.00-150.00   79
 19  \w   -118.00 -10.00   1.00    2.00    --  -42.16 -77.00 -60.00  108
;
_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      -0.1461805000
_diffrn_orient_matrix_UB_12      -0.0256186000
_diffrn_orient_matrix_UB_13      -0.0287466000
_diffrn_orient_matrix_UB_21      0.0165591000
_diffrn_orient_matrix_UB_22      0.0967510000
_diffrn_orient_matrix_UB_23      -0.0432238000
_diffrn_orient_matrix_UB_31      0.0400187000
_diffrn_orient_matrix_UB_32      -0.0928743000
_diffrn_orient_matrix_UB_33      -0.0515405000
_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  0.0223
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27568
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.031
_diffrn_reflns_theta_min         3.918
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.948
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.549
_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    1.537
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.178
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         9383
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0412
_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^)+(0.0533P)^2^+1.4436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1106
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8852
_reflns_number_total             9383
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-100-002y_200_red_ref
_cod_database_code               1566398
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C46 H38 P2 F12 N14'
_chemical_oxdiff_usercomment     '200 K'
_reflns_odcompleteness_completeness 99.81
_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-C45A \\sim N14B-C46B
 with sigma of 0.02
 N14A-C46A \\sim N14B-C45B
 with sigma of 0.02
 N13A-C36A \\sim N13B-C35B
 with sigma of 0.02
 N13A-C35A \\sim N13B-C36B
 with sigma of 0.02
 C45A-C43A \\sim C46B-C44B
 with sigma of 0.02
 C42A-C44A \\sim C42B-C43B
 with sigma of 0.02
 C42A-C43A \\sim C42B-C44B
 with sigma of 0.02
 C42A-C41A \\sim C42B-C41B
 with sigma of 0.02
 C46A-C44A \\sim C45B-C43B
 with sigma of 0.02
 C36A-C38A \\sim C35B-C37B
 with sigma of 0.02
 C39A-C38A \\sim C39B-C37B
 with sigma of 0.02
 C39A-C37A \\sim C39B-C38B
 with sigma of 0.02
 C39A-C40A \\sim C39B-C40B
 with sigma of 0.02
 C35A-C37A \\sim C36B-C38B
 with sigma of 0.02
 C40A-C41A \\sim C40B-C41B
 with sigma of 0.02
 N14A-C44A \\sim N14B-C43B
 with sigma of 0.04
 N14A-C43A \\sim N14B-C44B
 with sigma of 0.04
 N13A-C38A \\sim N13B-C37B
 with sigma of 0.04
 N13A-C37A \\sim N13B-C38B
 with sigma of 0.04
 C45A-C42A \\sim C46B-C42B
 with sigma of 0.04
 C45A-C46A \\sim C46B-C45B
 with sigma of 0.04
 C42A-C46A \\sim C42B-C45B
 with sigma of 0.04
 C42A-C40A \\sim C42B-C40B
 with sigma of 0.04
 C44A-C43A \\sim C43B-C44B
 with sigma of 0.04
 C44A-C41A \\sim C43B-C41B
 with sigma of 0.04
 C36A-C39A \\sim C35B-C39B
 with sigma of 0.04
 C36A-C35A \\sim C35B-C36B
 with sigma of 0.04
 C43A-C41A \\sim C44B-C41B
 with sigma of 0.04
 C39A-C35A \\sim C39B-C36B
 with sigma of 0.04
 C39A-C41A \\sim C39B-C41B
 with sigma of 0.04
 C38A-C37A \\sim C37B-C38B
 with sigma of 0.04
 C38A-C40A \\sim C37B-C40B
 with sigma of 0.04
 C37A-C40A \\sim C38B-C40B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C41A) = Uanis(N14A) = Uanis(C45A) = Uanis(C46A) = Uanis(C43A) =
Uanis(C44A) = Uanis(C42A) = Uanis(C40A) = Uanis(C39A) = Uanis(C38A) =
Uanis(C37A) = Uanis(C36A) = Uanis(C35A) = Uanis(N13A) = Uanis(C41B) =
Uanis(C39B) = Uanis(C40B) = Uanis(C37B) = Uanis(C38B) = Uanis(C35B) =
Uanis(C36B) = Uanis(C42B) = Uanis(N13B) = Uanis(C44B) = Uanis(C43B) =
Uanis(C46B) = Uanis(C45B) = Uanis(N14B)
4. Others
 Sof(C39B)=Sof(N14B)=Sof(C46B)=Sof(H46B)=Sof(C45B)=Sof(H45B)=Sof(C44B)=
 Sof(H44B)=Sof(C43B)=Sof(H43B)=Sof(C42B)=Sof(C41B)=Sof(H41B)=Sof(C40B)=
 Sof(H40B)=Sof(C37B)=Sof(H37B)=Sof(C38B)=Sof(H38B)=Sof(C35B)=Sof(H35B)=
 Sof(C36B)=Sof(H36B)=Sof(N13B)=1-FVAR(1)
 Sof(N14A)=Sof(N13A)=Sof(C45A)=Sof(H45A)=Sof(C42A)=Sof(C46A)=Sof(H46A)=
 Sof(C44A)=Sof(H44A)=Sof(C36A)=Sof(H36A)=Sof(C43A)=Sof(H43A)=Sof(C39A)=
 Sof(C35A)=Sof(H35A)=Sof(C38A)=Sof(H38A)=Sof(C37A)=Sof(H37A)=Sof(C40A)=
 Sof(H40A)=Sof(C41A)=Sof(H41A)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 N6(H6), N10(H10), N1(H1), N5(H5), C18(H18), C17(H17), C16(H16), C2(H2),
 C12(H12), C5(H5A), C13(H13), C7(H7), C6(H6A), C31(H31), C28(H28), C10(H10A),
 C21(H21), C1(H1A), C22(H22), C29(H29), C32(H32), C11(H11), C23(H23), C33(H33),
 C34(H34), C25(H25), C24(H24), C45A(H45A), C26(H26), C46A(H46A), C44A(H44A),
 C36A(H36A), C43A(H43A), C35A(H35A), C38A(H38A), C37A(H37A), C40A(H40A),
 C41A(H41A), C46B(H46B), C45B(H45B), C44B(H44B), C43B(H43B), C41B(H41B),
 C40B(H40B), C37B(H37B), C38B(H38B), C35B(H35B), C36B(H36B)
;
_shelx_res_checksum              31905
_shelx_hkl_checksum              12875
_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 1.295
_oxdiff_exptl_absorpt_empirical_full_min 0.832