Research on single-crystal-to-single-crystal photoaddition and extension of Schmidt's rule in topological chemistry
Xiao, Cheng-Yue; Deng, Xi-Ling; Wei, Zan-Bin; Yang, Shi-Yao; CrystEngComm 25 (2023) 3714–3717; doi:10.1039/D3CE00443K

data_7246937
_publ_section_title
;
 Research on single-crystal-to-single-crystal photoaddition and extension
 of Schmidt's rule in topological chemistry
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              3714
_journal_page_last               3717
_journal_paper_doi               10.1039/D3CE00443K
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety
'C29 H20.65 N2 O7 Zn2, 3.25(H2 O1), H0.6 O0.5, H0.5 O0.45, 0.25(O), 1.15(H), H0.4 O0.45'
_chemical_formula_sum            'C29 H29.8 N2 O11.9 Zn2'
_chemical_formula_weight         727.49
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-04-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-04-24 deposited with the CCDC.	2023-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                80.100(2)
_cell_angle_beta                 87.289(2)
_cell_angle_gamma                67.583(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3510(2)
_cell_length_b                   9.9976(2)
_cell_length_c                   18.0428(4)
_cell_measurement_reflns_used    18508
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.8230
_cell_measurement_theta_min      2.4960
_cell_volume                     1535.78(6)
_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)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34341
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.700
_diffrn_reflns_theta_max         75.302
_diffrn_reflns_theta_min         2.486
_exptl_absorpt_coefficient_mu    2.496
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             746
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.465
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         6003
_refine_ls_number_restraints     230
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0738P)^2^+6.0308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1435
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5462
_reflns_number_total             6003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00443k2.cif
_cod_data_source_block           y
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7246935--7246938.cif.
;
_cod_original_formula_sum        'C29 H29.80 N2 O11.90 Zn2'
_cod_database_code               7246937
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.788
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O7-H7
 0.85 with sigma of 0.01
 O1W-H1WA = O1W-H1WB = O2W-H2WA = O2W-H2WB = O3W-H3WA = O3W-H3WB
 0.85 with sigma of 0.01
 H1WA-H1WB = H2WA-H2WB = H3WA-H3WB
 1.38 with sigma of 0.01
 O4W-H4WA = O4W-H4WB = O5W-H5WA = O5W-H5WB = O6W-H6WA = O6W-H6WB
 0.85 with sigma of 0.01
 H4WA-H4WB = H5WA-H5WB = H6WA-H6WB
 1.38 with sigma of 0.01
 O7W-H7WA = O7W-H7WB = O8W-H8WA = O8W-H8WB = O9W-H9WA = O9W-H9WB
 0.85 with sigma of 0.01
 H7WA-H7WB = H8WA-H8WB = H9WA-H9WB
 1.38 with sigma of 0.01
 O16W-H16W = O16W-H15W = O17W-H17A = O17W-H17B = O18W-H18A = O18W-H18B
 0.85 with sigma of 0.01
 H16W-H15W = H17A-H17B = H18A-H18B
 1.38 with sigma of 0.01
 O19W-H19A = O19W-H19B = O20W-H20A = O20W-H20B
 0.85 with sigma of 0.01
 H19A-H19B = H20A-H20B
 1.38 with sigma of 0.01
 C23'-C24'
 1.34 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
N1 \\sim N1': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C10 \\sim C10': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C11 \\sim C11': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C12 \\sim C12': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C13 \\sim C13': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C14 \\sim C14': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C15 \\sim C15': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C16 \\sim C16': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C17 \\sim C17': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C18 \\sim C18': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C19 \\sim C19': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C20 \\sim C20': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C21 \\sim C21': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C22 \\sim C22': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C23 \\sim C23': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C24 \\sim C24': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C25 \\sim C25': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C26 \\sim C26': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C27 \\sim C27': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C28 \\sim C28': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C29 \\sim C29': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
N2 \\sim N2': within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
4. Same fragment restrains
{N1, C10, C11, C12, C13, C14, C15, C16, C17, C18, C19, C20, C21, C22, C23, C24,
C25, C26, C27, C28, C29, N2} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N1', C10', C11', C12', C13', C14', C15', C16', C17', C18', C19', C20', C21',
C22', C23', C24', C25', C26', C27', C28', C29', N2'}
5. Others
 Sof(N1')=Sof(C10')=Sof(H10')=Sof(C11')=Sof(H11')=Sof(C12')=Sof(C13')=
 Sof(H13')=Sof(C14')=Sof(H14')=Sof(C15')=Sof(H15')=Sof(C16')=Sof(H16')=
 Sof(C17')=Sof(C18')=Sof(H18')=Sof(C19')=Sof(H19')=Sof(C20')=Sof(C21')=
 Sof(H21')=Sof(C22')=Sof(H22')=Sof(C23')=Sof(H23')=Sof(C24')=Sof(H24')=
 Sof(C25')=Sof(C26')=Sof(H26')=Sof(C27')=Sof(H27')=Sof(C28')=Sof(H28')=
 Sof(C29')=Sof(H29')=Sof(N2')=1-FVAR(1)
 Sof(N1)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(C13)=Sof(H13)=
 Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(C18)=
 Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=
 Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(C26)=Sof(H26)=Sof(C27)=
 Sof(H27)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29)=Sof(N2)=FVAR(1)
 Fixed Sof: O1W(0.7) H1WA(0.7) H1WB(0.7) O2W(0.3) H2WA(0.3) H2WB(0.3)
 O3W(0.25) H3WA(0.25) H3WB(0.25) O4W(0.3) H4WA(0.3) H4WB(0.3) O5W(0.25)
 H5WA(0.25) H5WB(0.25) O6W(0.2) H6WA(0.2) H6WB(0.2) O7W(0.35) H7WA(0.35)
 H7WB(0.35) O8W(0.3) H8WA(0.3) H8WB(0.3) O9W(0.25) H9WA(0.25) H9WB(0.25)
 O10W(0.25) H(0.25) HA(0.25) O11W(0.2) HB(0.2) HC(0.2) O13W(0.2) HD(0.2)
 HE(0.2) O15W(0.25) HF(0.25) HG(0.25) O16W(0.2) H16W(0.2) H15W(0.2) O17W(0.2)
 H17A(0.2) H17B(0.2) O18W(0.3) H18A(0.3) H18B(0.3) O19W(0.2) H19A(0.2)
 H19B(0.2) O20W(0.2) H20A(0.2) H20B(0.2)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26),
  C27(H27), C28(H28), C29(H29), C10'(H10'), C11'(H11'), C13'(H13'), C14'(H14'),
 C15'(H15'), C16'(H16'), C18'(H18'), C19'(H19'), C21'(H21'), C22'(H22'),
 C23'(H23'), C24'(H24'), C26'(H26'), C27'(H27'), C28'(H28'), C29'(H29')
;
_shelx_res_checksum              29043
_shelx_hkl_checksum              63157
_olex2_submission_special_instructions 'No special instructions were received'