Diastereoselective solid-state crossed photocycloaddition of olefins in a 3D Zn(ii) coordination polymer.
Volodin, Alexander D.; Korlyukov, Alexander A.; Zorina-Tikhonova, Ekaterina N; Chistyakov, Aleksandr S.; Sidorov, Aleksei A.; Eremenko, Igor L.; Vologzhanina, Anna V.; Chemical communications (Cambridge, England) 54 (2018) 13861–13864; doi:10.1039/c8cc07734g

data_7122598
_publ_section_title
;
 Diastereoselective solid-state crossed photocycloaddition of olefins in a
 3D Zn(ii) coordination polymer.
;
_journal_issue                   98
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13861
_journal_page_last               13864
_journal_paper_doi               10.1039/c8cc07734g
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         '0.5(C48 H52 N4 O20 Zn4)'
_chemical_formula_sum            'C24 H26 N2 O10 Zn2'
_chemical_formula_weight         633.21
_chemical_properties_physical    Photo-sensitive
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-02-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2018-09-18 deposited with the CCDC.
2018-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 134.2590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.1598(5)
_cell_length_b                   24.1618(15)
_cell_length_c                   10.4735(7)
_cell_measurement_reflns_used    5265
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.66
_cell_measurement_theta_min      2.84
_cell_volume                     1297.63(15)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8827
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.661
_diffrn_reflns_theta_min         2.843
_exptl_absorpt_coefficient_mu    1.908
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0818 before and 0.0290 after correction.
The Ratio of minimum to maximum transmission is 0.7026.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_description       prism
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3982
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+1.2150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3654
_reflns_number_total             3982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07734g2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7122598--7122601.cif.'
_cod_database_code               7122598
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O5-H5A
 0.87 with sigma of 0.02
3.a Rotating group:
 O5(H5A,H5B)
3.b Ternary CH refined with riding coordinates:
 C2(H2)
3.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
3.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12)
3.e X=CH2 refined with riding coordinates:
 C6(H6A,H6B)
;
_shelx_res_checksum              64935
_olex2_submission_special_instructions 'No special instructions were received'