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_1566394
_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(C10 H8 N4), 2(B F4)'
_chemical_formula_sum            'C42 H34 B2 F8 Fe N18'
_chemical_formula_weight         1020.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 97.592(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9764(2)
_cell_length_b                   18.0458(3)
_cell_length_c                   24.6253(4)
_cell_measurement_reflns_used    6910
_cell_measurement_temperature    80.0(6)
_cell_measurement_theta_max      71.8030
_cell_measurement_theta_min      4.4500
_cell_volume                     4394.48(14)
_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(6)
_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 0.965
_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    -46.00 -18.00   1.00    1.00    --  -42.16 -38.00-180.00   28
  2  \w    -64.00 -20.00   1.00    1.00    --  -42.16 -38.00   0.00   44
  3  \w   -122.00  -2.00   1.00    1.00    --  -42.16 -19.00 -90.00  120
  4  \w     48.00  89.00   1.00    1.00    --   42.16-125.00  30.00   41
  5  \w     24.00  81.00   1.00    4.00    --  103.72 -94.00-120.00   57
  6  \w    124.00 163.00   1.00    4.00    --  103.72  61.00-180.00   39
  7  \w     64.00 113.00   1.00    4.00    --  103.72 -61.00 -90.00   49
  8  \w    140.00 172.00   1.00    4.00    --  103.72 125.00 -60.00   32
  9  \w     94.00 120.00   1.00    4.00    --  103.72 125.00 -60.00   26
 10  \w     35.00 128.00   1.00    4.00    --  103.72 -30.00  90.00   93
 11  \w    123.00 177.00   1.00    4.00    --  103.72 125.00  60.00   54
 12  \w     35.00 136.00   1.00    4.00    --  103.72 -77.00  30.00  101
;
_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      0.0194644000
_diffrn_orient_matrix_UB_12      0.0535235000
_diffrn_orient_matrix_UB_13      0.0491933000
_diffrn_orient_matrix_UB_21      -0.0665742000
_diffrn_orient_matrix_UB_22      -0.0567560000
_diffrn_orient_matrix_UB_23      0.0346774000
_diffrn_orient_matrix_UB_31      0.1394431000
_diffrn_orient_matrix_UB_32      -0.0347290000
_diffrn_orient_matrix_UB_33      0.0189941000
_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  0.0309
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            18282
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.443
_diffrn_reflns_theta_min         3.622
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.548
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.406
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       block
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.133
_refine_diff_density_max         1.824
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         8412
_refine_ls_number_restraints     169
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0530
_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^)+(0.0850P)^2^+3.3615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1501
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7143
_reflns_number_total             8412
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-115-002r_80_red_ref
_cod_database_code               1566394
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C42 H34 N18 B2 F8'
_chemical_oxdiff_usercomment     '80  K'
_reflns_odcompleteness_completeness 99.95
_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
 F2A-B1A \\sim F2B-B1B
 with sigma of 0.02
 F1-B1A \\sim F1-B1B
 with sigma of 0.02
 F3A-B1A \\sim F3B-B1B
 with sigma of 0.02
 F4A-B1A \\sim F4B-B1B
 with sigma of 0.02
 F3A-F4A \\sim F3B-F4B
 with sigma of 0.04
 F1-F2A \\sim F1-F2B
 with sigma of 0.04
 F1-F3A \\sim F1-F3B
 with sigma of 0.04
 F1-F4A \\sim F1-F4B
 with sigma of 0.04
 F2A-F3A \\sim F2B-F3B
 with sigma of 0.04
 F2A-F4A \\sim F2B-F4B
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 B1A, F1, F2A, F3A, F4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B2, F6, F5, F7, F8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N14, N13, N12, C28, C27, C29, C30, C25, C26, H29, C31, H30, C32, H25, C23,
 H26, C24, H31, H32, N11, H23, H24
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(B1B)=Sof(F2B)=Sof(F4B)=Sof(F3B)=1-FVAR(1)
 Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(B1A)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 N5(H5), N10(H10), N6(H6), N1(H1), C16(H16), C7(H7), C13(H13), C6(H6a),
 C5(H5a), C18(H18), C17(H17), C21(H21), C12(H12), C42(H42), C10(H10a), C41(H41),
  C39(H39), C25(H25), C2(H2), C1(H1a), C11(H11), C26(H26), C40(H40), C22(H22),
 C29(H29), C36(H36), C23(H23), C34(H34), C30(H30), C33(H33), C24(H24), C31(H31),
  C35(H35), C32(H32)
;
_shelx_res_checksum              19247
_shelx_hkl_checksum              4596
_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 1.150
_oxdiff_exptl_absorpt_empirical_full_min 0.893