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_1566379
_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      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 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-11 deposited with the CCDC.	2022-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                82.284(4)
_cell_angle_beta                 82.051(4)
_cell_angle_gamma                87.374(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2090(4)
_cell_length_b                   10.4618(5)
_cell_length_c                   21.8559(10)
_cell_measurement_reflns_used    5737
_cell_measurement_temperature    270.00(17)
_cell_measurement_theta_max      71.7660
_cell_measurement_theta_min      4.2390
_cell_volume                     2290.06(18)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      270.00(17)
_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 0.968
_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    2.00    --  -42.16  57.00-120.00  101
  2  \w    -92.00  -2.00   1.00    2.00    --  -42.16 125.00 -60.00   90
  3  \w   -108.00 -14.00   1.00    2.00    --  -42.16 -57.00  90.00   94
  4  \w     22.00 115.00   1.00    2.00    --   42.16  38.00   0.00   93
  5  \w     34.00 121.00   1.00   12.00    --  103.72 -45.00-150.00   87
  6  \w     31.00  64.00   1.00   12.00    --  103.72 -61.00  60.00   33
  7  \w     53.00 108.00   1.00   12.00    --  103.72 -94.00  60.00   55
  8  \w     57.00  83.00   1.00   12.00    --  103.72 -94.00 150.00   26
  9  \w    118.00 168.00   1.00   12.00    --  103.72  61.00   0.00   50
 10  \w     38.00 128.00   1.00   12.00    --  103.72 -45.00 -60.00   90
 11  \w     41.00 130.00   1.00   12.00    --  103.72 -45.00  60.00   89
 12  \w     28.00 118.00   1.00   12.00    --  103.72 -77.00-150.00   90
 13  \w     67.00 117.00   1.00   12.00    --  103.72-125.00-120.00   50
 14  \w     71.00 115.00   1.00   12.00    --  103.72-125.00  30.00   44
 15  \w     22.00  49.00   1.00   12.00    --  103.72 -94.00  60.00   27
 16  \w     16.00 172.00   1.00   12.00    --  103.72   0.00   0.00  156
;
_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      -0.0611763000
_diffrn_orient_matrix_UB_12      -0.0037920000
_diffrn_orient_matrix_UB_13      0.0687047000
_diffrn_orient_matrix_UB_21      -0.0645232000
_diffrn_orient_matrix_UB_22      0.1345239000
_diffrn_orient_matrix_UB_23      -0.0150394000
_diffrn_orient_matrix_UB_31      -0.1238054000
_diffrn_orient_matrix_UB_32      -0.0631526000
_diffrn_orient_matrix_UB_33      -0.0143156000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16932
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.186
_diffrn_reflns_theta_min         4.119
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.404
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.489
_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    1.480
_exptl_crystal_description       plate
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.037
_refine_diff_density_max         1.109
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         8758
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0732
_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^)+(0.1389P)^2^+1.0914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2090
_refine_ls_wR_factor_ref         0.2253
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7145
_reflns_number_total             8758
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-115-002y_270_red_ref
_cod_database_code               1566379
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C42 H34 N18 B2 F8'
_chemical_oxdiff_usercomment     '270 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
 F5-B2 \\sim F6-B2 \\sim F7-B2 \\sim F8-B2
 with sigma of 0.002
 F8-F5 \\sim F6-F7
 with sigma of 0.002
3. Rigid body (RIGU) restrains
 B1, F4, F1, F3, F2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B2, F8, F7, F5, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N18, N16, N17, C37, C38, C35, C36, C40, C39, C33, H35, H36, C34, H40, C42,
 C41, H39, H33, N15, H34, H42, H41
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Aromatic/amide H refined with riding coordinates:
 N6(H6), N1(H1), N10(H10), N5(H5), C16(H16), C18(H18), C12(H12), C13(H13),
 C17(H17), C22(H22), C21(H21), C5(H5A), C7(H7), C6(H6A), C33(H33), C29(H29),
 C35(H35), C36(H36), C2(H2), C25(H25), C1(H1A), C30(H30), C34(H34), C23(H23),
 C40(H40), C41(H41), C32(H32), C24(H24), C31(H31), C39(H39), C11(H11),
 C10(H10A), C26(H26), C42(H42)
;
_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 1.092
_oxdiff_exptl_absorpt_empirical_full_min 0.933