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_7122599
_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             2018-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-31 deposited with the CCDC.
2018-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 134.60(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.227(13)
_cell_length_b                   25.30(4)
_cell_length_c                   10.480(18)
_cell_measurement_reflns_used    1814
_cell_measurement_temperature    375
_cell_measurement_theta_max      23.51
_cell_measurement_theta_min      2.93
_cell_volume                     1364(4)
_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      375
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_unetI/netI     0.0913
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12500
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.576
_diffrn_reflns_theta_min         2.846
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.815
_exptl_absorpt_correction_T_max  0.3368
_exptl_absorpt_correction_T_min  0.2622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1069 before and 0.0637 after correction.
The Ratio of minimum to maximum transmission is 0.7785.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.542
_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         0.496
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         4101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0520P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1301
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2365
_reflns_number_total             4101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07734g2.cif
_cod_data_source_block           fin375
_cod_depositor_comments
'Adding full bibliography for 7122598--7122601.cif.'
_cod_database_code               7122599
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.621
_shelx_estimated_absorpt_t_min   0.446
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H4AA(0.5) H4AB(0.5) H4BC(0.5) H4BD(0.5) C5(0.5) H5(0.5) C5A(0.5)
 H5AA(0.5) C6(0.5) H6A(0.5) H6B(0.5) C6A(0.5) H6AA(0.5) H6AB(0.5)
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(H4AA,H4AB), C4(H4BC,H4BD)
3.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C5A(H5AA)
3.e X=CH2 refined with riding coordinates:
 C6(H6A,H6B), C6A(H6AA,H6AB)
;
_shelx_res_checksum              81016
_olex2_submission_special_instructions 'No special instructions were received'