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_1566399
_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      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-03 deposited with the CCDC.	2022-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.403(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2076(3)
_cell_length_b                   18.9941(9)
_cell_length_c                   22.8634(8)
_cell_measurement_reflns_used    5682
_cell_measurement_temperature    300.0(2)
_cell_measurement_theta_max      71.7920
_cell_measurement_theta_min      4.4920
_cell_volume                     4405.2(3)
_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_environment      air
_diffrn_ambient_temperature      300.0(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 0.982
_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   -116.00 -17.00   1.00    5.00    --  -41.91 -38.00-180.00   99
  2  \w    -92.00  -2.00   1.00    5.00    --  -41.91 125.00 -30.00   90
  3  \w      9.00 118.00   1.00    5.00    --   41.91  77.00 120.00  109
  4  \w     27.00 132.00   1.00   20.00    --  103.72 -30.00-180.00  105
  5  \w     31.00 118.00   1.00   20.00    --  103.72-125.00-180.00   87
  6  \w     31.00 130.00   1.00   20.00    --  103.72 -45.00 -90.00   99
  7  \w     94.00 177.00   1.00   20.00    --  103.72 125.00-180.00   83
  8  \w     31.00 130.00   1.00   20.00    --  103.72 -45.00  90.00   99
  9  \w     97.00 174.00   1.00   20.00    --  103.72  45.00-180.00   77
 10  \w     43.00 130.00   1.00   20.00    --  103.72 -77.00  90.00   87
;
_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      -0.0729265000
_diffrn_orient_matrix_UB_12      -0.0608448000
_diffrn_orient_matrix_UB_13      -0.0343779000
_diffrn_orient_matrix_UB_21      -0.0438176000
_diffrn_orient_matrix_UB_22      0.0506758000
_diffrn_orient_matrix_UB_23      -0.0510153000
_diffrn_orient_matrix_UB_31      0.1257820000
_diffrn_orient_matrix_UB_32      -0.0175552000
_diffrn_orient_matrix_UB_33      -0.0285402000
_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  0.0476
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25065
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.973
_diffrn_reflns_theta_min         3.891
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.477
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.302
_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    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.143
_refine_diff_density_max         2.814
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         8525
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.0982
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2572
_refine_ls_wR_factor_ref         0.2914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5993
_reflns_number_total             8525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-137-001_300ah_red_ref
_cod_database_code               1566399
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C42 H34 N14 B2 F8'
_chemical_oxdiff_usercomment     '300 K After heating to 400 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 N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N5(H5), N6(H6), N1(H1), N10(H10), C7(H7), C16(H16), C5(H5a), C18(H18),
 C10(H10a), C6(H6a), C17(H17), C25(H25), C11(H11), C26(H26), C13(H13), C12(H12),
  C2(H2), C36(H36), C40(H40), C42(H42), C30(H30), C29(H29), C35(H35), C32(H32),
 C23(H23), C24(H24), C31(H31), C1(H1a), C21(H21), C33(H33), C34(H34), C22(H22),
 C41(H41), C39(H39)
;
_shelx_res_checksum              59562
_shelx_hkl_checksum              54062
_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 1.229
_oxdiff_exptl_absorpt_empirical_full_min 0.817