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_1566387
_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(B F4), 2(C10 H8 N2)'
_chemical_formula_sum            'C42 H34 B2 F8 Fe N14'
_chemical_formula_weight         964.30
_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                96.133(3)
_cell_angle_beta                 94.628(3)
_cell_angle_gamma                93.979(4)
_cell_formula_units_Z            2
_cell_length_a                   10.2254(4)
_cell_length_b                   10.1492(6)
_cell_length_c                   21.6116(6)
_cell_measurement_reflns_used    6419
_cell_measurement_temperature    330.00(15)
_cell_measurement_theta_max      71.4770
_cell_measurement_theta_min      4.0940
_cell_volume                     2215.84(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)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      330.00(15)
_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 0.969
_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  -6.00   1.00    1.50    --  -42.16 125.00  90.00   86
  2  \w   -112.00 -18.00   1.00    1.50    --  -42.16 -57.00-120.00   94
  3  \w    -64.00  29.00   1.00    1.50    --  -42.16  57.00  30.00   93
  4  \w    -57.00  31.00   1.00    1.50    --  -42.16  38.00-180.00   88
  5  \w     29.00  95.00   1.00    6.00    --  103.72 -94.00 150.00   66
  6  \w     41.00 107.00   1.00    6.00    --  103.72 -94.00  60.00   66
  7  \w    118.00 164.00   1.00    6.00    --  103.72  45.00 -30.00   46
  8  \w     32.00 117.00   1.00    6.00    --  103.72-125.00  30.00   85
  9  \w     75.00 172.00   1.00    6.00    --  103.72  61.00-150.00   97
 10  \w     78.00 104.00   1.00    6.00    --  103.72  61.00-180.00   26
 11  \w    119.00 168.00   1.00    6.00    --  103.72  61.00-180.00   49
 12  \w     71.00 171.00   1.00    6.00    --  103.72  77.00  90.00  100
 13  \w    121.00 173.00   1.00    6.00    --  103.72 125.00  60.00   52
 14  \w     78.00 104.00   1.00    6.00    --  103.72  30.00 -60.00   26
 15  \w    142.00 171.00   1.00    6.00    --  103.72  30.00 -60.00   29
 16  \w     95.00 156.00   1.00    6.00    --  103.72 125.00  30.00   61
 17  \w     33.00 118.00   1.00    6.00    --  103.72-125.00 -90.00   85
 18  \w     31.00  75.00   1.00    6.00    --  103.72 -77.00   0.00   44
;
_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      -0.0792272056
_diffrn_orient_matrix_UB_12      -0.1356625162
_diffrn_orient_matrix_UB_13      -0.0030924640
_diffrn_orient_matrix_UB_21      0.1292717899
_diffrn_orient_matrix_UB_22      -0.0688203433
_diffrn_orient_matrix_UB_23      0.0063487711
_diffrn_orient_matrix_UB_31      -0.0013440592
_diffrn_orient_matrix_UB_32      0.0176424627
_diffrn_orient_matrix_UB_33      0.0716315980
_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  0.0398
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16626
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.062
_diffrn_reflns_theta_min         4.131
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.456
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.137
_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    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.366
_exptl_crystal_size_mid          0.348
_exptl_crystal_size_min          0.246
_refine_diff_density_max         0.908
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         8476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0719
_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^)+(0.1202P)^2^+0.5191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2011
_refine_ls_wR_factor_ref         0.2128
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6971
_reflns_number_total             8476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-106-002b_330_reduap_ref
_cod_original_cell_volume        2215.84(16)
_cod_database_code               1566387
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C42 H34 B2 F8 N14'
_chemical_oxdiff_usercomment     '330 K'
_reflns_odcompleteness_completeness 99.97
_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.a Aromatic/amide H refined with riding coordinates:
 N5(H5), N6(H6), N1(H1), N10(H10), C18(H18), C17(H17), C16(H16), C7(H7),
 C10(H10A), C13(H13), C5(H5A), C11(H11), C6(H6A), C12(H12), C2(H2), C29(H29),
 C36(H36), C26(H26), C31(H31), C30(H30), C35(H35), C39(H39), C21(H21), C1(H1A),
 C32(H32), C41(H41), C25(H25), C24(H24), C40(H40), C22(H22), C34(H34), C33(H33),
  C23(H23), C42(H42)
;
_shelx_res_checksum              87899
_shelx_hkl_checksum              35733
_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 1.466
_oxdiff_exptl_absorpt_empirical_full_min 0.739