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_1566386
_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 H10 N2)'
_chemical_formula_sum            'C46 H38 B2 F8 Fe N14'
_chemical_formula_weight         1016.37
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-09
_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                 99.669(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4294(5)
_cell_length_b                   18.5284(11)
_cell_length_c                   24.7378(8)
_cell_measurement_reflns_used    3180
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.0110
_cell_measurement_theta_min      4.2700
_cell_volume                     4712.4(4)
_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_temperature      293(2)
_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 0.981
_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  -2.00   1.00   10.00    --  -42.16 125.00 120.00   90
  2  \w   -116.00 -18.00   1.00   10.00    --  -42.16 -38.00 -60.00   98
  3  \w    -92.00  -2.00   1.00   10.00    --  -42.16 125.00  90.00   90
  4  \w     31.00 118.00   1.00   40.00    --  103.72-125.00 -90.00   87
  5  \w     31.00 118.00   1.00   40.00    --  103.72-125.00  30.00   87
  6  \w     78.00 177.00   1.00   40.00    --  103.72  45.00 -30.00   99
  7  \w    100.00 175.00   1.00   40.00    --  103.72 125.00-180.00   75
  8  \w     94.00 120.00   1.00   40.00    --  103.72 125.00-120.00   26
  9  \w    144.00 171.00   1.00   40.00    --  103.72 125.00-120.00   27
 10  \w     21.00  81.00   1.00   40.00    --  103.72 -94.00 -60.00   60
 11  \w     21.00  54.00   1.00   40.00    --  103.72 -94.00-150.00   33
 12  \w     36.00 129.00   1.00   40.00    --  103.72 -30.00  30.00   93
;
_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      -0.0482404000
_diffrn_orient_matrix_UB_12      -0.0686121000
_diffrn_orient_matrix_UB_13      0.0255349000
_diffrn_orient_matrix_UB_21      0.1333984000
_diffrn_orient_matrix_UB_22      -0.0358405000
_diffrn_orient_matrix_UB_23      0.0003086000
_diffrn_orient_matrix_UB_31      0.0482049000
_diffrn_orient_matrix_UB_32      0.0304392000
_diffrn_orient_matrix_UB_33      0.0577704000
_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  0.0583
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25171
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.946
_diffrn_reflns_theta_min         3.625
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.281
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.846
_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    1.433
_exptl_crystal_description       plate
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.097
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         9068
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0614
_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^)+(0.0679P)^2^+1.0318P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5430
_reflns_number_total             9068
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-106-003a_rt_red_ref
_cod_database_code               1566386
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C46 H38 B2 F8 N14'
_chemical_oxdiff_usercomment     RT
_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
 F1-F4A \\sim F1-F2A \\sim F1-F3A \\sim F4A-F2A \\sim F4A-F3A \\sim F2A-F3A
 with sigma of 0.04
 B1-F1 \\sim B1-F4A \\sim B1-F2A \\sim B1-F3A
 with sigma of 0.02
 C40B-C39 \\sim C40A-C39 \\sim C41A-C42 \\sim C41B-C42
 with sigma of 0.02
 F2B-F4B \\sim F2B-F3B \\sim F3A-F2A \\sim F2A-F4A
 with sigma of 0.04
 B1-F2B \\sim B1-F4B \\sim B1-F3A \\sim B1-F2A \\sim B1-F1 \\sim B1-F4A \\sim
B1-F3B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C40A) = Uanis(C40B)
Uanis(C41A) = Uanis(C41B)
Uanis(F3A) = Uanis(F2B)
Uanis(F2A) = Uanis(F4B)
Uanis(F4A) = Uanis(F3B)
4. Rigid body (RIGU) restrains
 B1, F1, F2B, F4B, F3A, F2A, F4A, F3B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C40B)=Sof(H40B)=Sof(C41B)=Sof(H41B)=1-FVAR(1)
 Sof(C40A)=Sof(H40A)=Sof(C41A)=Sof(H41A)=FVAR(1)
 Sof(F2B)=Sof(F4B)=Sof(F3B)=1-FVAR(2)
 Sof(F4A)=Sof(F2A)=Sof(F3A)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N6(H6), N5(H5), N10(H10), C12(H12), C29(H29), C2(H2), C1(H1A),
 C31(H31), C7(H7), C18(H18), C11(H11), C21(H21), C10(H10A), C5(H5A), C32(H32),
 C28(H28), C24(H24), C16(H16), C17(H17), C26(H26), C25(H25), C13(H13), C22(H22),
  C6(H6A), C23(H23), C34(H34), C33(H33), C46(H46), C38(H38), C36(H36), C35(H35),
  C37(H37), C44(H44), C45(H45), C43(H43), C40A(H40A), C41A(H41A), C40B(H40B),
 C41B(H41B)
;
_shelx_res_checksum              33078
_shelx_hkl_checksum              86811
_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 1.216
_oxdiff_exptl_absorpt_empirical_full_min 0.893