Synthesis and luminescence properties of functionalized V-shaped bis-coumarin derivatives
Su, Ruige; Zhao, Yuling; Liu, Shiqiang; Li, Peiying; Ma, Jiaying; Zhang, Di; Han, Minghu; Yu, Tianzhi; New Journal of Chemistry 46 (2022) 6793–6803; doi:10.1039/D1NJ05960B

data_7061372
_publ_section_title
;
 Synthesis and luminescence properties of functionalized V-shaped
 bis-coumarin derivatives
;
_journal_issue                   14
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6793
_journal_page_last               6803
_journal_paper_doi               10.1039/D1NJ05960B
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C32 H24 N2 O4'
_chemical_formula_sum            'C32 H24 N2 O4'
_chemical_formula_weight         500.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-16
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.09.11 svn.r3730fd0d for OlexSys, GUI svn.r6159)
;
_audit_update_record
;
2021-10-06 deposited with the CCDC.	2022-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                107.530(7)
_cell_angle_beta                 98.155(5)
_cell_angle_gamma                110.522(6)
_cell_formula_units_Z            2
_cell_length_a                   9.0562(5)
_cell_length_b                   11.4544(10)
_cell_length_c                   13.3288(9)
_cell_measurement_reflns_used    3025
_cell_measurement_temperature    149.98(10)
_cell_measurement_theta_max      28.6170
_cell_measurement_theta_min      2.4580
_cell_volume                     1186.42(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -14.00  78.00   1.00    1.00    --   11.90  77.00 -30.00   92
  2  \w     63.00  89.00   1.00    1.00    --   11.90 178.00  60.00   26
  3  \w    -39.00  55.00   1.00    1.00    --  -11.27  57.00-150.00   94
  4  \w    -83.00  12.00   1.00    1.00    --  -11.27 -57.00  60.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0632051000
_diffrn_orient_matrix_UB_12      -0.0661317000
_diffrn_orient_matrix_UB_13      -0.0259788000
_diffrn_orient_matrix_UB_21      0.0121885000
_diffrn_orient_matrix_UB_22      -0.0102223000
_diffrn_orient_matrix_UB_23      0.0498836000
_diffrn_orient_matrix_UB_31      -0.0585830000
_diffrn_orient_matrix_UB_32      0.0250024000
_diffrn_orient_matrix_UB_33      0.0144977000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8323
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         2.051
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_description       block
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         4173
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0475P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1158
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3071
_reflns_number_total             4173
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj05960b1.cif
_cod_data_source_block           cz
_cod_depositor_comments
'Adding full bibliography for 7061372--7061373.cif.'
_cod_original_cell_volume        1186.41(16)
_cod_database_code               7061372
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 N2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C31, C32
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C32) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C31) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C31) = Uanis(C34)
4. Others
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=1-FVAR(1)
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C31(H31A,H31B), C33(H33A,H33B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C18(H18), C25(H25), C27(H27)
5.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              68614
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.288
_oxdiff_exptl_absorpt_empirical_full_min 0.615