Polymorph driven diversification of photosalient responses in a zinc(II) coordination complex.
Pham-Tran, Victoria N P; Moffat, James G. D.; Marczenko, Katherine M.; Chemical communications (Cambridge, England) 60 (2024) 7890–7893; doi:10.1039/d4cc01593b

data_7133257
_publ_section_title
;
 Polymorph driven diversification of photosalient responses in a zinc(II)
 coordination complex.
;
_journal_issue                   61
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              7890
_journal_page_last               7893
_journal_paper_doi               10.1039/d4cc01593b
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C48 H36 N2 O6 Zn'
_chemical_formula_sum            'C48 H36 N2 O6 Zn'
_chemical_formula_weight         802.16
_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             2024-06-07
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-09 deposited with the CCDC.	2024-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.802(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9164(2)
_cell_length_b                   23.6249(8)
_cell_length_c                   20.5918(6)
_cell_measurement_reflns_used    7015
_cell_measurement_temperature    292.7(3)
_cell_measurement_theta_max      23.5010
_cell_measurement_theta_min      2.0070
_cell_volume                     3849.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.121a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.121a 64-bit (release 24-04-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.121a (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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.7(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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    -30.00  66.00   0.50   25.00    --   20.00  54.00-120.00  192
  2  \w    -71.00  26.00   0.50   25.00    --   20.00  54.00  30.00  194
  3  \w     44.00 110.00   0.50   25.00    --   20.00  54.00  30.00  132
  4  \w    -73.00 -25.00   0.50   25.00    --   20.00  54.00 120.00   96
  5  \w      7.00  34.00   0.50   25.00    --   20.00  54.00 120.00   54
  6  \w     41.00  66.00   0.50   25.00    --   20.00  54.00 120.00   50
  7  \w    -35.00  82.00   0.50   25.00    --   20.00  54.00 -30.00  234
  8  \w      3.00  26.00   0.50   25.00    --   20.00  54.00 -90.00   46
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0871963000
_diffrn_orient_matrix_UB_12      -0.0025020000
_diffrn_orient_matrix_UB_13      -0.0063519000
_diffrn_orient_matrix_UB_21      0.0076029000
_diffrn_orient_matrix_UB_22      -0.0221214000
_diffrn_orient_matrix_UB_23      0.0232051000
_diffrn_orient_matrix_UB_31      -0.0191921000
_diffrn_orient_matrix_UB_32      -0.0201539000
_diffrn_orient_matrix_UB_33      -0.0246842000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27701
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.413
_diffrn_reflns_theta_min         1.988
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.693
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.947
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.121a (Rigaku Oxford Diffraction, 2024)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.491
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         7862
_refine_ls_number_restraints     550
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0497P)^2^+1.1523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5348
_reflns_number_total             7862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01593b2.cif
_cod_data_source_block           1-form-iii-prime
_cod_depositor_comments
'Adding full bibliography for 7133256--7133260.cif.'
_cod_database_code               7133257
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         ZnC30H30N2O6
_chemical_oxdiff_usercomment     'after 30 sec UV exposure 10 Watt'
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.727
_olex2_refinement_description
;
1. Restrained distances
 C5A-C4A = C4A-C3A = C3A-C2A = C2A-C1A
 1.39 with sigma of 0.01
 C5A-C3A \\sim C4A-C2A \\sim C3A-C1A \\sim C1A-C5A
 with sigma of 0.02
 C9A-C10A \\sim C11A-C10A \\sim C12A-C11A \\sim C9A-C8A \\sim C8A-C17A \\sim
C17A-C12A \\sim C15A-C14A
 \\sim C16A-C15A \\sim C17A-C16A
 with sigma of 0.02
 C16A-C15A \\sim C17A-C16A \\sim C15A-C14A \\sim C17A-C12A
 with sigma of 0.02
 C15A-C12A \\sim C17A-C14A
 with sigma of 0.02
 C17A-C10A \\sim C8A-C11A \\sim C12A-C9A
 with sigma of 0.02
 N1-C5 \\sim N1-C1
 with sigma of 0.02
 C13-C12 \\sim C14-C13
 with sigma of 0.02
 N1A-C1A \\sim N1A-C5A
 with sigma of 0.02
 C14A-C13 \\sim C13-C12A
 with sigma of 0.02
2. Restrained planarity
 N1A, C1A, C2A, C3A, C4A, C5A
 with sigma of 0.1
 C9A, C10A, C11A, C12A, C14A, C15A, C16A, C17A
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
N1A \\sim C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim
C8A \\sim C9A \\sim C10A \\sim C11A \\sim C12A \\sim C14A \\sim C15A \\sim C16A
\\sim C17A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N1A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(C4A)=Sof(H4A)=
 Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6AA)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(C9A)=
 Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H13A)=Sof(C14A)=
 Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=1-FVAR(1)
 Sof(N1)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(C4)=Sof(H4)=Sof(C5)=
 Sof(H5)=Sof(C6)=Sof(H6A)=Sof(C7)=Sof(H7)=Sof(C8)=Sof(C9)=Sof(H9)=Sof(C10)=
 Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C15)=
 Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C6A(H6AA), C7A(H7A)
6.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C47(H47), C48(H48), C45(H45), C44(H44), C37(H37), C38(H38),
 C40(H40), C1(H1), C1A(H1A), C2(H2), C2A(H2A), C4(H4), C4A(H4A), C5(H5),
 C5A(H5A), C6(H6A), C7(H7), C9(H9), C9A(H9A), C10(H10), C10A(H10A), C11(H11),
 C11A(H11A), C13(H13), C13(H13A), C14(H14), C14A(H14A), C15(H15), C15A(H15A),
 C16(H16), C16A(H16A), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23),
 C24(H24), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33)
6.c Idealised tetrahedral OH refined as rotating group:
 O3(H3), O6(H6)
;
_shelx_res_checksum              9349
_shelx_hkl_checksum              2206
_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 1.302
_oxdiff_exptl_absorpt_empirical_full_min 0.810