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_7122601
_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_absolute_configuration ad
_chemical_formula_moiety         'C24 H26 N2 O10 Zn2'
_chemical_formula_sum            'C24 H26 N2 O10 Zn2'
_chemical_formula_weight         633.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-22 deposited with the CCDC.
2018-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.750(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.1981(9)
_cell_length_b                   24.070(3)
_cell_length_c                   7.4585(9)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.57
_cell_measurement_theta_min      2.86
_cell_volume                     1292.1(3)
_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_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            21602
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.617
_diffrn_reflns_theta_min         0.846
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.916
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_description       prism
_exptl_crystal_F_000             648
_exptl_crystal_recrystallization_method
'The complex was obtained in the course of photoreaction'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.484
_refine_diff_density_min         -2.918
_refine_diff_density_rms         0.191
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         7852
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      0.008
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0843
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.067
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+17.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1880
_refine_ls_wR_factor_ref         0.1980
_reflns_Friedel_coverage         0.991
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                6543
_reflns_number_total             7852
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07734g2.cif
_cod_data_source_block           a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7122598--7122601.cif.'
_cod_database_code               7122601
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.607
_shelx_estimated_absorpt_t_min   0.479
_olex2_refinement_description
;
1. Others
 Fixed Sof: H4BC(0.25) H4BD(0.25) H4AA(0.75) H4AB(0.75) Zn2A(0.75) O6A(0.75)
 O7A(0.75) O8A(0.75) O9A(0.75) O10A(0.75) H10A(0.75) H10B(0.75) C7A(0.75)
 H7A(0.75) C8A(0.75) H8A(0.75) C9A(0.75) C19A(0.75) C20A(0.75) H20A(0.75)
 C21A(0.75) C22A(0.75) H22A(0.75) H22B(0.75) C23A(0.75) H23A(0.75) C24A(0.75)
 H24A(0.75) H24B(0.75) Zn2B(0.25) O6B(0.25) O7B(0.25) O8B(0.25) O9B(0.25)
 O10B(0.25) H10C(0.25) H10D(0.25) C5B(0.25) H5BA(0.25) C6B(0.25) H6BA(0.25)
 H6BB(0.25) C9B(0.25) C8B(0.25) H8B(0.25) C7B(0.25) H7B(0.25) H10(0.75)
 H10E(0.25) C19B(0.25) C20B(0.25) H20B(0.25) C21B(0.25) C22B(0.25) H22C(0.25)
 H22D(0.25) C23B(0.25) H23B(0.25) C24B(0.25) H24C(0.25) H24D(0.25) C3AA(0.25)
 H3AA(0.25) C2AA(0.75) H2AA(0.75) C1AA(0.75) H1AA(0.75) C0AA(0.75) H0AA(0.75)
 C6(0.25) H6(0.25) C7(0.75) H7C(0.75) H7D(0.75) C17A(0.75) H17A(0.75)
 C18A(0.75) H18A(0.75) N2A(0.75) C14A(0.75) H14A(0.75) C15A(0.75) H15A(0.75)
 N2B(0.25) C14B(0.25) H14B(0.25) C15B(0.25) H15B(0.25) C17B(0.25) H17B(0.25)
 C18B(0.25) H18B(0.25)
 Fixed Uiso: H5A(0.022) H5B(0.022) H2(0.023) H4BC(0.048) H4BD(0.048)
 H4AA(0.048) H4AB(0.048) H10A(0.103) H10B(0.103) H7A(0.066) H8A(0.08)
 H20A(0.073) H22A(0.113) H22B(0.113) H23A(0.113) H24A(0.113) H24B(0.113)
 H10C(0.094) H10D(0.094) H5BA(0.037) H6BA(0.068) H6BB(0.068) H8B(0.08)
 H7B(0.066) H11(0.04) H10(0.051) H10E(0.051) H20B(0.066) H22C(0.113)
 H22D(0.113) H23B(0.113) H24C(0.113) H24D(0.113) H3AA(0.136) H2AA(0.136)
 H1AA(0.136) H0AA(0.136) H6(0.136) H7C(0.136) H7D(0.136) H17A(0.083)
 H18A(0.069) H14A(0.085) H15A(0.086) H14B(0.058) H15B(0.086) H17B(0.059)
 H18B(0.087)
 Fixed X: H5A(-0.6988) H5B(-0.89) H2(-0.2945) H4BC(-0.427) H4BD(-0.2632) H4AA(-
 0.2976) H4AB(-0.1812) H10A(-0.8828) H10B(-0.7265) H7A(-0.7178) H8A(-0.5671)
 H20A(-0.7849) H22A(-0.9299) H22B(-0.7214) H23A(-0.6819) H24A(-0.8193) H24B(-
 0.7274) H10C(-0.6193) H10D(-0.5001) H5BA(-0.1505) H6BA(-0.1294) H6BB(-0.0285)
 H8B(-0.7335) H7B(-0.76) H11(-0.811) H10(-0.8472) H10E(-0.7845) H20B(-0.6007)
 H22C(-0.4737) H22D(-0.6807) H23B(-0.3871) H24C(-0.6362) H24D(-0.4559) H3AA(-
 0.8021) H2AA(-0.6846) H1AA(-0.5486) H0AA(-0.4437) H6(-0.6638) H7C(-0.2892)
 H7D(-0.4794) H17A(-0.6578) H18A(-0.7747) H14A(-0.7952) H15A(-0.6782) H14B(-
 0.6574) H15B(-0.694) H17B(-0.5943) H18B(-0.5577)
 Fixed Y: H5A(-0.5208) H5B(-0.5203) H2(-0.4006) H4BC(-0.3399) H4BD(-0.3611)
 H4AA(-0.3622) H4AB(-0.3338) H10A(0.0217) H10B(0.0266) H7A(-0.3437) H8A(-
 0.2829) H20A(0.0987) H22A(0.1562) H22B(0.1497) H23A(0.1851) H24A(0.2573)
 H24B(0.2802) H10C(0.0654) H10D(0.0339) H5BA(-0.3108) H6BA(-0.2715) H6BB(-
 0.2461) H8B(-0.2685) H7B(-0.3395) H11(-0.4528) H10(-0.3754) H10E(-0.3818)
 H20B(0.0885) H22C(0.1489) H22D(0.1653) H23B(0.1929) H24C(0.2753) H24D(0.2794)
 H3AA(-0.2844) H2AA(-0.2906) H1AA(-0.3248) H0AA(-0.2213) H6(-0.2184) H7C(-
 0.2448) H7D(-0.2385) H17A(-0.1333) H18A(-0.0584) H14A(-0.1554) H15A(-0.2302)
 H14B(-0.1487) H15B(-0.2233) H17B(-0.1205) H18B(-0.046)
 Fixed Z: H5A(-2.3793) H5B(-2.3793) H2(-1.5577) H4BC(-1.3274) H4BD(-1.1983)
 H4AA(-1.1951) H4AB(-1.3509) H10A(-0.8209) H10B(-0.7778) H7A(-2.1102) H8A(-
 1.8842) H20A(-1.1452) H22A(-1.4025) H22B(-1.4721) H23A(-1.1215) H24A(-1.4083)
 H24B(-1.2192) H10C(-0.8683) H10D(-0.7743) H5BA(-1.5179) H6BA(-1.1759) H6BB(-
 1.3549) H8B(-1.9188) H7B(-2.1321) H11(-1.7338) H10(-1.5364) H10E(-1.5205)
 H20B(-1.0983) H22C(-1.3989) H22D(-1.3565) H23B(-1.128) H24C(-1.2247) H24D(-
 1.0874) H3AA(-1.4497) H2AA(-1.4536) H1AA(-1.2708) H0AA(-1.6236) H6(-1.7237)
 H7C(-1.3527) H7D(-1.2418) H17A(-1.6523) H18A(-1.4885) H14A(-1.0449) H15A(-
 1.2087) H14B(-1.0346) H15B(-1.2333) H17B(-1.6516) H18B(-1.4529)
;
_shelx_res_checksum              47562
_olex2_submission_special_instructions 'No special instructions were received'