Rh(i)-Catalyzed intramolecular [2 + 2 + 1] cycloaddition of diynes with the N-terminal of the diazo group
Wang, Bo; Wang, Yuankai; Wang, Zixuan; Wang, Jianbo; Organic Chemistry Frontiers 6 (2019) 2329–; doi:10.1039/C9QO00403C

data_1554903
_publ_section_title
;
 Rh(i)-Catalyzed intramolecular [2 + 2 + 1] cycloaddition of diynes with
 the N-terminal of the diazo group
;
_journal_issue                   14
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              2329
_journal_paper_doi               10.1039/C9QO00403C
_journal_volume                  6
_journal_year                    2019
_chemical_formula_sum            'C19 H20 N2 O3'
_chemical_formula_weight         324.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-03-13 deposited with the CCDC.	2019-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.405(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.5666(3)
_cell_length_b                   16.4713(6)
_cell_length_c                   8.0376(4)
_cell_measurement_reflns_used    3032
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      28.8470
_cell_measurement_theta_min      2.7190
_cell_volume                     809.39(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      180.00(10)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5239
_diffrn_reflns_point_group_measured_fraction_full 0.739
_diffrn_reflns_point_group_measured_fraction_max 0.636
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.261
_diffrn_reflns_theta_min         2.473
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       block
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.142
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 663 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.2(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2802
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0513P)^2^+0.0107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0880
_reflns_Friedel_coverage         0.353
_reflns_Friedel_fraction_full    0.459
_reflns_Friedel_fraction_max     0.343
_reflns_number_gt                2586
_reflns_number_total             2802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9qo00403c2.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1554903
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              59344
_shelx_hkl_checksum              99999