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_1566395
_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(C12 H12 N2)'
_chemical_formula_sum            'C46 H42 F12 Fe N14 P2'
_chemical_formula_weight         1136.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_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                 102.668(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0523(3)
_cell_length_b                   30.8080(9)
_cell_length_c                   18.3037(9)
_cell_measurement_reflns_used    11988
_cell_measurement_temperature    135.00(13)
_cell_measurement_theta_max      71.8750
_cell_measurement_theta_min      3.7610
_cell_volume                     4980.3(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      N~2~
_diffrn_ambient_temperature      135.00(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 0.989
_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    -66.00  32.00   1.00    3.00    --  -41.91  38.00 150.00   98
  2  \w   -115.00 -17.00   1.00    3.00    --  -41.91 -38.00 -30.00   98
  3  \w    -82.00  13.00   1.00    3.00    --  -41.91 106.00-130.00   95
  4  \w    -18.00  16.00   1.00    3.00    --   41.91 -38.00-180.00   34
  5  \w     59.00  88.00   1.00    3.00    --   41.91-125.00  90.00   29
  6  \w     35.00 126.00   1.00   12.00    --  103.72 -30.00  90.00   91
  7  \w     98.00 178.00   1.00   12.00    --  103.72  30.00 120.00   80
  8  \w     35.00 108.00   1.00   12.00    --  103.72 -61.00  90.00   73
  9  \w     31.00 111.00   1.00   12.00    --  103.72-125.00 -90.00   80
 10  \w     32.00  78.00   1.00   12.00    --  103.72 -45.00-150.00   46
 11  \w     34.00 123.00   1.00   12.00    --  103.72 -61.00 -60.00   89
 12  \w    110.00 175.00   1.00   12.00    --  103.72 125.00  60.00   65
 13  \w     30.00 109.00   1.00   12.00    --  103.72 -94.00  90.00   79
 14  \w     76.00 127.00   1.00   12.00    --  103.72 -77.00 150.00   51
 15  \w     22.00 150.00   1.00   12.00    --  103.72 -15.00 -60.00  128
 16  \w     82.00 118.00   1.00   12.00    --  103.72-125.00  90.00   36
 17  \w     87.00 114.00   1.00   12.00    --  103.72-125.00   0.00   27
;
_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      -0.0353802000
_diffrn_orient_matrix_UB_12      -0.0483954000
_diffrn_orient_matrix_UB_13      0.0086050000
_diffrn_orient_matrix_UB_21      -0.1052315000
_diffrn_orient_matrix_UB_22      0.0001936000
_diffrn_orient_matrix_UB_23      -0.0785673000
_diffrn_orient_matrix_UB_31      0.1346898000
_diffrn_orient_matrix_UB_32      -0.0125599000
_diffrn_orient_matrix_UB_33      -0.0345025000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21662
_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         72.107
_diffrn_reflns_theta_min         3.790
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.881
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.486
_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    1.516
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.179
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.002(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1352
_refine_ls_number_reflns         21662
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0839P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.1367
_reflns_Friedel_coverage         0.946
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.974
_reflns_number_gt                17644
_reflns_number_total             21662
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9884\% 
 around [0.91 -0.00 -0.41] (reciprocal) or [1.00 0.00 0.00] (direct)
;
_cod_data_source_file            d1sc04956a1.cif
_cod_data_source_block           ltb-103-002_135_mptwinred_twin1_hklf4
_cod_database_code               1566395
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Fe C46 H38 P2 F12 N14'
_chemical_oxdiff_usercomment     '135 K'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5620(12)
 0.4380(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
3.a Secondary CH2 refined with riding coordinates:
 C86(H86a,H86b), C62(H62a,H62b), C75(H75a,H75b), C74(H74a,H74b), C51(H51a,
 H51b), C87(H87a,H87b), C50(H50a,H50b), C63(H63a,H63b)
3.b Aromatic/amide H refined with riding coordinates:
 N6(H6), N15(H15), N11(H11a), N1(H1), N5(H5), N20(H20), C13(H13), N16(H16a),
 C38(H38), C84(H84), C29(H29), N10(H10), C89(H89), C45(H45), C16(H16), C53(H53),
  C92(H92), C35(H35), C48(H48), C12(H12), C78(H78), C68(H68), C83(H83),
 C43(H43), C55(H55), C2(H2), C46(H46), C47(H47), C10(H10a), C7(H7), C91(H91),
 C17(H17), C22(H22), C34(H34), C54(H54), C69(H69), C11(H11), C71(H71), C5(H5a),
 C82(H82), C33(H33), C44(H44), C27(H27), C70(H70), C1(H1a), C6(H6a), C90(H90),
 C18(H18), C28(H28), C40(H40), C59(H59), C80(H80), C56(H56), C21(H21), C65(H65),
  C77(H77), C72(H72), C57(H57), C23(H23), C39(H39), C81(H81), C60(H60),
 C66(H66), C32(H32), C58(H58), C79(H79), C67(H67), C24(H24)
;
_shelx_res_checksum              56381
_shelx_hkl_checksum              69232
_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 1.351
_oxdiff_exptl_absorpt_empirical_full_min 0.789
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2