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_1566383
_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(C12 H12 N2)'
_chemical_formula_sum            'C46 H42 B2 F8 Fe N14'
_chemical_formula_weight         1020.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                 98.8910(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0537(2)
_cell_length_b                   9.57810(10)
_cell_length_c                   22.3969(3)
_cell_measurement_reflns_used    12667
_cell_measurement_temperature    149(1)
_cell_measurement_theta_max      72.9710
_cell_measurement_theta_min      3.9750
_cell_volume                     4674.11(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (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      149(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2887
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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    -70.00  31.00   1.00    5.00    --  -42.16  57.00-150.00  101
  2  \w   -116.00 -18.00   1.00    5.00    --  -42.16 -38.00 -60.00   98
  3  \w   -115.00 -14.00   1.00    5.00    --  -42.16 -57.00  60.00  101
  4  \w      1.00  83.00   1.00    5.00    --   42.16 -99.00 -60.00   82
  5  \w     77.00 178.00   1.00   20.00    --  105.91  61.00 -60.00  101
  6  \w     33.00 118.00   1.00   20.00    --  105.91-125.00-120.00   85
  7  \w     23.00 109.00   1.00   20.00    --  105.91 -94.00 -90.00   86
  8  \w     77.00 178.00   1.00   20.00    --  105.91  61.00-120.00  101
  9  \w     34.00 135.00   1.00   20.00    --  105.91 -61.00 -60.00  101
 10  \w     73.00 178.00   1.00   20.00    --  105.91  77.00 -90.00  105
 11  \w     23.00 109.00   1.00   20.00    --  105.91 -94.00  90.00   86
 12  \w     33.00 118.00   1.00   20.00    --  105.91-125.00  60.00   85
 13  \w     34.00 135.00   1.00   20.00    --  105.91 -61.00  90.00  101
 14  \w     94.00 178.00   1.00   20.00    --  105.91 125.00-180.00   84
 15  \w     34.00 135.00   1.00   20.00    --  105.91 -61.00-180.00  101
 16  \w     53.00 178.00   1.00   20.00    --  105.91  15.00  30.00  125
 17  \w   -118.00 -10.00   1.00    5.00    --  -42.16 -77.00 -90.00  108
 18  \w   -115.00 -14.00   1.00    5.00    --  -42.16 -57.00-180.00  101
 19  \w      1.00  75.00   1.00    5.00    --   42.16 -99.00  30.00   74
;
_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      0.0606732000
_diffrn_orient_matrix_UB_12      -0.0728679000
_diffrn_orient_matrix_UB_13      0.0259023000
_diffrn_orient_matrix_UB_21      0.0014416000
_diffrn_orient_matrix_UB_22      0.0805817000
_diffrn_orient_matrix_UB_23      0.0597328000
_diffrn_orient_matrix_UB_31      -0.0362817000
_diffrn_orient_matrix_UB_32      -0.1186239000
_diffrn_orient_matrix_UB_33      0.0246490000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25568
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.144
_diffrn_reflns_theta_min         3.996
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.308
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.515
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (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    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         4647
_refine_ls_number_restraints     200
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0460P)^2^+3.9802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4504
_reflns_number_total             4647
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-63-002_redmi_refprac
_cod_database_code               1566383
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C34 H40 N14 B2 F8'
_chemical_oxdiff_usercomment     '150 K'
_reflns_odcompleteness_completeness 99.96
_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 C(H,H) groups, All N(H) groups
2. Restrained distances
 C19-C18A \\sim C19-C18B
 with sigma of 0.02
 C16-C17A \\sim C16-C17B
 with sigma of 0.02
 C18A-C17A \\sim C18B-C17B
 with sigma of 0.02
 C19-C17A \\sim C19-C17B
 with sigma of 0.04
 C16-C18A \\sim C16-C18B
 with sigma of 0.04
 F2-F1 \\sim F3A-F4A \\sim F4B-F3B
 with sigma of 0.04
 B1-F2 \\sim B1-F1 \\sim B1-F3A \\sim B1-F4A \\sim B1-F4B \\sim B1-F3B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 F3A, F4A, B1, F2, F1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F4B, F3B, B1, F2, F1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C16, N7, C22, C23, H22, C20, C21, H23, C19, H20, H21, C18A, C18B, H18A, H18B,
 C17A, C17B, H18C, H18D, H17A, H17B, H17C, H17D, C14, C15, C12, H14, C13, H15,
 N6, H12, H13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15, N7, C22, C23, H22, C20, C21, H23, C19, H20, H21, C18A, C18B, H18A, H18B,
 C17A, C17B, H18C, H18D, C16, H17A, H17B, H17C, H17D, C14, C12, H14, C13, H15,
 N6, H12, H13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C17B)=Sof(H17C)=Sof(H17D)=Sof(C18B)=Sof(H18C)=Sof(H18D)=1-FVAR(1)
 Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(C17A)=Sof(H17A)=Sof(H17B)=FVAR(1)
 Sof(F4B)=Sof(F3B)=1-FVAR(2)
 Sof(F3A)=Sof(F4A)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C18A(H18A,H18B), C17A(H17A,H17B), C17B(H17C,H17D), C18B(H18C,H18D)
5.b Aromatic/amide H refined with riding coordinates:
 N5(H5), C5(H5A), C7(H7), C6(H6), C11(H11), C22(H22), C10(H10), C2(H2),
 C1(H1A), C20(H20), C21(H21), C23(H23), C12(H12), C13(H13), C14(H14), C15(H15)
;
_shelx_res_checksum              22655
_shelx_hkl_checksum              13717
_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 0.817