An acid-catalyzed 1,4-addition isocyanide-based multicomponent reaction in neat water
Lei, Jie; Li, Yong; Xu, Jia; Tang, Dian-Yong; Shao, Jing-Wei; Li, Hong-yu; Chen, Zhong-Zhu; Xu, Zhi-Gang; Green Chemistry 22 (2020) 3716–3720; doi:10.1039/D0GC00652A

data_7240682
_publ_section_title
;
 An acid-catalyzed 1,4-addition isocyanide-based multicomponent reaction
 in neat water
;
_journal_issue                   12
_journal_name_full               'Green Chemistry'
_journal_page_first              3716
_journal_page_last               3720
_journal_paper_doi               10.1039/D0GC00652A
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         'C33 H33 Cl N2 O4'
_chemical_formula_sum            'C33 H33 Cl N2 O4'
_chemical_formula_weight         557.09
_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_Int_Tables_number      14
_audit_creation_date             2019-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-13 deposited with the CCDC.	2020-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.155(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3143(11)
_cell_length_b                   13.9869(12)
_cell_length_c                   20.0442(9)
_cell_measurement_reflns_used    1298
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18.57
_cell_measurement_theta_min      2.47
_cell_volume                     2854.8(4)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.9982
_diffrn_measured_fraction_theta_max 0.9982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0956
_diffrn_reflns_av_unetI/netI     0.1476
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17576
_diffrn_reflns_theta_full        24.9998
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.78
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.2960
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1177.1279
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.4737
_refine_diff_density_min         -0.3730
_refine_diff_density_rms         0.0957
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             11.4219
_refine_ls_goodness_of_fit_ref   1.1102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    54
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1102
_refine_ls_R_factor_all          0.1463
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1398
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                2297
_reflns_number_total             5020
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0gc00652a2.cif
_cod_data_source_block           A
_cod_depositor_comments
;Adding full bibliography for 7240682.cif.

 Adding full bibliography for 7240682.cif.
;
_cod_database_code               7240682
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C20(H20)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C9(H9a,H9b)
2.c Me refined with riding coordinates:
 C13(H13a,H13b,H13c), C18(H18a,H18b,H18c), C31(H31a,H31b,H31c), C32(H32a,H32b,
 H32c), C33(H33a,H33b,H33c)
2.d Aromatic/amide H refined with riding coordinates:
 N2(H2), C2(H2a), C3(H3), C5(H5), C6(H6), C14(H14), C15(H15), C16(H16),
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29)
;
_olex2_submission_special_instructions 'No special instructions were received'