Controlled microcrystallization for in situ photocrystallography: optimizing crystal size and habit
Lewis, Sam G.; Coulson, Ben A.; Harris, Kenneth D. M.; Warren, Anna J.; Warren, Mark R.; Hatcher, Lauren E.; CrystEngComm 27 (2025) 4965–4975; doi:10.1039/D5CE00367A

data_7250589
_publ_section_title
;
 Controlled microcrystallization for in situ photocrystallography:
 optimizing crystal size and habit
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              4965
_journal_page_last               4975
_journal_paper_doi               10.1039/D5CE00367A
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C6 H6 Fe N6 Na2 O3'
_chemical_formula_sum            'C6 H6 Fe N6 Na2 O3'
_chemical_formula_weight         312.00
_chemical_properties_physical
Moisture-sensitive,Hygroscopic,Light-sensitive,Photo-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-11
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-04-01 deposited with the CCDC.	2025-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.462(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.9370(4)
_cell_length_b                   7.8904(2)
_cell_length_c                   24.4181(9)
_cell_measurement_reflns_used    4285
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.4340
_cell_measurement_theta_min      3.7500
_cell_volume                     2413.57(14)
_computing_cell_refinement       'CrysAlisPro 1.171.43.141a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.141a 64-bit (release 04-10-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.141a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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    102.00 158.00   0.50    0.58    --  107.00  30.00-120.00  112
  2  \w     96.00 130.00   0.50    0.58    --  107.00  30.00  30.00   68
  3  \w    144.00 169.00   0.50    0.58    --  107.00  30.00  30.00   50
  4  \w    128.00 176.00   0.50    0.58    --  107.00  30.00 150.00   96
  5  \w     96.00 123.00   0.50    0.58    --  107.00  30.00 150.00   54
  6  \w    100.00 177.00   0.50    0.58    --  107.00  15.00 -60.00  154
  7  \w     36.00  70.00   0.50    0.58    --  107.00 -77.00-120.00   68
  8  \w     84.00 109.00   0.50    0.58    --  107.00 -77.00-120.00   50
  9  \w     55.00  84.00   0.50    0.14    --   48.98-125.00-145.00   58
 10  \w     82.00 112.00   0.50    0.58    --  107.00-125.00-120.00   60
 11  \w     54.00  80.00   0.50    0.58    --  107.00-125.00-120.00   52
 12  \w     37.00  67.00   0.50    0.58    --  107.00 -95.00 -60.00   60
 13  \w     74.00 101.00   0.50    0.58    --  107.00 -95.00 -60.00   54
 14  \w     51.00  97.00   0.50    0.58    --  107.00 -95.00  60.00   92
 15  \w     69.00 112.00   0.50    0.58    --  107.00-125.00 120.00   86
 16  \w     35.00 106.00   0.50    0.58    --  107.00 -77.00 150.00  142
 17  \w   -113.00  -1.00   0.50    0.14    --  -48.98   0.00 -30.00  224
 18  \w    -27.00   1.00   0.50    0.14    --  -48.98  38.00 -30.00   56
 19  \w    -19.00  25.00   0.50    0.14    --  -48.98  19.00-180.00   88
 20  \w    -67.00 -32.00   0.50    0.58    -- -104.50  61.00   0.00   70
 21  \w   -173.00-136.00   0.50    0.58    -- -104.50 -15.00  30.00   74
 22  \w   -165.00-139.00   0.50    0.58    -- -104.50 -61.00 -60.00   52
 23  \w   -116.00 -90.00   0.50    0.58    -- -104.50 -61.00 -60.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
;
CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      0.1226267000
_diffrn_orient_matrix_UB_12      -0.0119311000
_diffrn_orient_matrix_UB_13      0.0195148000
_diffrn_orient_matrix_UB_21      -0.0053963000
_diffrn_orient_matrix_UB_22      0.0259718000
_diffrn_orient_matrix_UB_23      0.0617471000
_diffrn_orient_matrix_UB_31      -0.0081082000
_diffrn_orient_matrix_UB_32      -0.1931078000
_diffrn_orient_matrix_UB_33      0.0071477000
_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  0.0249
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            7110
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.077
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         3.739
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.863
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.141a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_description       plate
_exptl_crystal_F_000             1248
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol, ethanol'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2128
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0496P)^2^+3.6138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1900
_reflns_number_total             2128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00367a2.cif
_cod_data_source_block           SNP_H2O_MeOH_solvate
_cod_depositor_comments          'Adding full bibliography for 7250589.cif.'
_cod_database_code               7250589
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C6H6FeN6Na2O3
_chemical_oxdiff_usercomment     '100K collection of 311a'
_diffrn_oxdiff_digest_hkl
;
013e169c0a13caecaf2b87398c2dd8a5191077
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H2A,H2B,H3} of C6
 At 1.5 times of:
  {H6A,H6B,H6C} of C6
2. Restrained distances
 O3-H3
 0.95 with sigma of 0.02
 H2A-O2
 0.95 with sigma of 0.02
 O2-H2B
 0.95 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4.a Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_shelx_res_checksum              38401
_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 2.078
_oxdiff_exptl_absorpt_empirical_full_min 0.641