Iodine catalyzed one-pot four component synthesis of coumarinyl phosphoramidates via sequential addition of reactants
Imrankhan, Mohammed; Shivashankar, Kalegowda; New Journal of Chemistry 44 (2020) 18573–18578; doi:10.1039/D0NJ04445H

data_7060025
_publ_section_title
;
 Iodine catalyzed one-pot four component synthesis of coumarinyl
 phosphoramidates via sequential addition of reactants
;
_journal_issue                   43
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18573
_journal_page_last               18578
_journal_paper_doi               10.1039/D0NJ04445H
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C14 H18 N O5 P'
_chemical_formula_sum            'C14 H18 N O5 P'
_chemical_formula_weight         311.26
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2019-02-12 deposited with the CCDC.	2020-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                99.987(6)
_cell_angle_beta                 100.884(6)
_cell_angle_gamma                103.517(6)
_cell_formula_units_Z            4
_cell_length_a                   7.4224(12)
_cell_length_b                   14.193(2)
_cell_length_c                   17.094(3)
_cell_measurement_reflns_used    4477
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.25
_cell_volume                     1674.2(5)
_computing_cell_refinement       'SAINT (Bruker,1998)'
_computing_data_collection       'SMART (Bruker,1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2009)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX CCD detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36364
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    0.183
_exptl_absorpt_correction_T_max  0.9731
_exptl_absorpt_correction_T_min  0.9714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS  (Bruker, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.597
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.949
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.949
_refine_ls_R_factor_all          0.1576
_refine_ls_R_factor_gt           0.1381
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.041
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4180
_refine_ls_wR_factor_ref         0.4399
_reflns_number_gt                4477
_reflns_number_total             5896
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            d0nj04445h2.cif
_cod_data_source_block           red
_cod_depositor_comments
;
       Adding full bibliography for 7060025.cif.

2024-06-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     'C28 H36 N2 O10 P2'
_cod_original_formula_sum        'C28 H36 N2 O10 P2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     622.53
_cod_database_code               7060025