Efficient synthesis of new asymmetric tripodal ligands using microwave irradiation, and their crystal structures
Yuan, Zeli; Yang, Xiaoqing; Wang, Lei; Huang, Jiandong; Wei, Gang; RSC Adv. 4 (2014) 42211–; doi:10.1039/C4RA07346K

data_7218078
_publ_section_title
;
 Efficient synthesis of new asymmetric tripodal ligands using microwave
 irradiation, and their crystal structures
;
_journal_issue                   79
_journal_name_full               'RSC Adv.'
_journal_page_first              42211
_journal_paper_doi               10.1039/C4RA07346K
_journal_volume                  4
_journal_year                    2014
_chemical_formula_sum            'C23 H21 N3 O'
_chemical_formula_weight         355.43
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.512(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.929(10)
_cell_length_b                   12.099(12)
_cell_length_c                   16.261(16)
_cell_measurement_temperature    293(2)
_cell_volume                     1941(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12490
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.9857
_exptl_absorpt_correction_T_min  0.9827
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.207
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.030(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0999P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1410
_refine_ls_wR_factor_ref         0.1533
_reflns_number_gt                2267
_reflns_number_total             3386
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra07346k3.cif
_cod_data_source_block           yzl
_cod_database_code               7218078