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_1566392
_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(F6 P), 2(C10 H8 N2)'
_chemical_formula_sum            'C42 H34 F12 Fe N14 P2'
_chemical_formula_weight         1080.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_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                 95.4899(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.9529(3)
_cell_length_b                   14.8247(3)
_cell_length_c                   21.0093(3)
_cell_measurement_reflns_used    6715
_cell_measurement_temperature    298.00(13)
_cell_measurement_theta_max      71.8650
_cell_measurement_theta_min      4.2000
_cell_volume                     4635.82(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (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      air
_diffrn_ambient_temperature      298.00(13)
_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 0.987
_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    -27.00  -2.00   1.00    1.00    --  -42.16 125.00-180.00   25
  2  \w    -87.00 -59.00   1.00    1.00    --  -42.16 125.00-180.00   28
  3  \w   -115.00 -19.00   1.00    1.00    --  -42.16 -38.00  60.00   96
  4  \w   -116.00 -18.00   1.00    1.00    --  -42.16 -38.00 150.00   98
  5  \w      2.00  80.00   1.00    1.00    --   42.16 -99.00  30.00   78
  6  \w     29.00  56.00   1.00    1.00    --   42.16-125.00 -30.00   27
  7  \w      3.00  46.00   1.00    1.00    --   42.16 -99.00 -60.00   43
  8  \w     31.00  82.00   1.00    4.00    --  103.72 -61.00  90.00   51
  9  \w     33.00  58.00   1.00    4.00    --  103.72-125.00 -90.00   25
 10  \w     64.00 107.00   1.00    4.00    --  103.72 -94.00  90.00   43
 11  \w     94.00 127.00   1.00    4.00    --  103.72 125.00  30.00   33
 12  \w     75.00 118.00   1.00    4.00    --  103.72-125.00 -90.00   43
 13  \w     39.00  66.00   1.00    4.00    --  103.72 -45.00 -60.00   27
 14  \w     37.00 118.00   1.00    4.00    --  103.72-125.00  60.00   81
 15  \w     75.00 137.00   1.00    4.00    --  103.72  61.00  90.00   62
 16  \w     97.00 166.00   1.00    4.00    --  103.72 125.00-180.00   69
 17  \w    119.00 177.00   1.00    4.00    --  103.72 125.00 -60.00   58
 18  \w     44.00 116.00   1.00    4.00    --  103.72 -30.00-150.00   72
 19  \w    107.00 133.00   1.00    4.00    --  103.72 -61.00  90.00   26
 20  \w     30.00 117.00   1.00    4.00    --  103.72 -77.00-120.00   87
 21  \w     51.00 178.00   1.00    4.00    --  103.72  15.00-150.00  127
;
_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      -0.0445973000
_diffrn_orient_matrix_UB_12      -0.0775932000
_diffrn_orient_matrix_UB_13      -0.0402356000
_diffrn_orient_matrix_UB_21      0.0075887000
_diffrn_orient_matrix_UB_22      -0.0611760000
_diffrn_orient_matrix_UB_23      0.0595574000
_diffrn_orient_matrix_UB_31      -0.0930664000
_diffrn_orient_matrix_UB_32      0.0321731000
_diffrn_orient_matrix_UB_33      0.0162513000
_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  0.0287
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17455
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.043
_diffrn_reflns_theta_min         4.209
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.138
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.341
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (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    1.548
_exptl_crystal_description       block
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.134
_refine_diff_density_max         1.039
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4687
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0623
_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^)+(0.1351P)^2^+2.5431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1888
_refine_ls_wR_factor_ref         0.1981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4072
_reflns_number_total             4687
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-97-002r_298_red_ref
_cod_original_cell_volume        4635.81(15)
_cod_database_code               1566392
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C42 H34 P2 F12 N14'
_chemical_oxdiff_usercomment     '298 K Red crystal'
_reflns_odcompleteness_completeness 99.98
_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. Rigid body (RIGU) restrains
 P2, F6, F5, F7, F8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P1, F3, F2, F1, F4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N4(H4), N8(H8), C5(H5), C6(H6), C13(H13), C2(H2), C1(H1A), C11(H11),
 C8(H8A), C12(H12), C16(H16), C17(H17), C7(H7), C19(H19), C22(H22), C18(H18),
 C23(H23), C26(H26), C27(H27), C24(H24), C25(H25)
;
_shelx_res_checksum              22474
_shelx_hkl_checksum              33545
_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 0.872