The synthesis and photophysical properties of tris-coumarins.
Kielesiński, Łukasz; Morawski, Olaf W.; Sobolewski, Andrzej L.; Gryko, Daniel T.; Physical chemistry chemical physics : PCCP 21 (2019) 8314–8325; doi:10.1039/c9cp00978g

data_1550826
_publ_section_title
;
 The synthesis and photophysical properties of tris-coumarins.
;
_journal_issue                   16
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              8314
_journal_page_last               8325
_journal_paper_doi               10.1039/c9cp00978g
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C39 H33 N3 O9, C H Cl3'
_chemical_formula_sum            'C40 H34 Cl3 N3 O9'
_chemical_formula_weight         807.05
_chemical_melting_point_gt       573
_chemical_name_systematic        Cy-3Amide-7
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_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-2014
_audit_update_record
;
2019-02-15 deposited with the CCDC.    2019-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                81.027(2)
_cell_angle_beta                 74.327(2)
_cell_angle_gamma                61.2690(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7636(3)
_cell_length_b                   13.1274(3)
_cell_length_c                   14.2142(3)
_cell_measurement_reflns_used    2175
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      66.42
_cell_measurement_theta_min      3.23
_cell_volume                     2009.81(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.839
_diffrn_measured_fraction_theta_max 0.862
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_unetI/netI     0.1480
_diffrn_reflns_Laue_measured_fraction_full 0.839
_diffrn_reflns_Laue_measured_fraction_max 0.862
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            48013
_diffrn_reflns_point_group_measured_fraction_full 0.839
_diffrn_reflns_point_group_measured_fraction_max 0.862
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.422
_diffrn_reflns_theta_min         3.231
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.547
_exptl_absorpt_correction_T_max  0.9300
_exptl_absorpt_correction_T_min  0.8200
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             836
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane/chloroform'
_exptl_crystal_size_max          0.286
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0009(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   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         6109
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.2579
_refine_ls_R_factor_gt           0.0938
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0881P)^2^+4.2061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2177
_refine_ls_wR_factor_ref         0.2875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2175
_reflns_number_total             6109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cp00978g2.cif
_cod_data_source_block           LK297_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_melting_point_gt' since the value was specified as 'more
than' ('>') a certain temperature. The value '>573' was changed to
'573' - it should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 1550826.cif.
;
_cod_database_code               1550826
_shelx_estimated_absorpt_t_min   0.530
_shelx_estimated_absorpt_t_max   0.781
_shelxl_version_number           2014-3
_shelx_res_checksum              13194
_shelx_hkl_checksum              13506