Domino aza/oxa-hetero-Diels–Alder reaction for construction of novel spiro[pyrido[3′,2′:5,6]pyrano[2,3-d]pyrimidine-7,5′-pyrimidine]
Yang, Wen-Juan; Sun, Qiu; Sun, Jing; Yan, Chao-Guo; Organic Chemistry Frontiers 5 (2018) 2754–; doi:10.1039/C8QO00784E

data_1554411
_publ_section_title
;
 Domino aza/oxa-hetero-Diels--Alder reaction for construction of novel
 spiro[pyrido[3&#x2032;,2&#x2032;:5,6]pyrano[2,3-d]pyrimidine-7,5&#x2032;-pyrimidine]
;
_journal_issue                   18
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              2754
_journal_paper_doi               10.1039/C8QO00784E
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         'C42 H38 Cl N5 O6'
_chemical_formula_sum            'C42 H38 Cl N5 O6'
_chemical_formula_weight         744.22
_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   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-07-25 deposited with the CCDC.
2018-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                96.558(9)
_cell_angle_beta                 109.996(8)
_cell_angle_gamma                107.812(9)
_cell_formula_units_Z            2
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_cell_length_b                   12.455(3)
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_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.67
_cell_measurement_theta_min      2.44
_cell_volume                     2236.9(10)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2020
_diffrn_reflns_av_unetI/netI     0.2734
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
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_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
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_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        24.713
_diffrn_reflns_theta_max         24.713
_diffrn_reflns_theta_min         1.930
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7441
_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.2438
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_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1486P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2511
_refine_ls_wR_factor_ref         0.3034
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3191
_reflns_number_total             7441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qo00784e2.cif
_cod_data_source_block           5a
_cod_original_cell_volume        2236.8(9)
_cod_database_code               1554411
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.966
_shelx_estimated_absorpt_t_max   0.977
_shelx_res_checksum              5369
_shelx_hkl_checksum              325
_shelx_fab_checksum              21748