Copper-mediated phospha-annulation to attain water-soluble polycyclic luminophores
Belyaev, Andrey; Chen, Yi-Ting; Su, Shih-Hao; Tseng, Yu-Jui; Karttunen, Antti J.; Tunik, Sergey P.; Chou, Pi-Tai; Koshevoy, Igor O.; Chem. Commun.  (2017) –; doi:10.1039/C7CC06882D

data_7120701
_publ_section_title
;
 Copper-mediated phospha-annulation to attain water-soluble polycyclic
 luminophores
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC06882D
_journal_year                    2017
_chemical_formula_moiety         'C52 H42 P2, 2(I)'
_chemical_formula_sum            'C52 H42 I2 P2'
_chemical_formula_weight         982.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-07-24 deposited with the CCDC.
2017-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.6523(9)
_cell_length_b                   12.2403(5)
_cell_length_c                   13.5209(5)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.23
_cell_measurement_theta_min      2.38
_cell_volume                     4245.5(3)
_computing_cell_refinement       'SAINT (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_molecular_graphics    'Diamond v.4.03 (Brandenburg, 2014)'
_computing_publication_material  'SHELXL-2016 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '62mm x 62mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Bruker KAPPA APEX II DUO CCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offset'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48631
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.380
_diffrn_reflns_theta_min         1.588
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.593
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.082
_refine_diff_density_max         1.219
_refine_diff_density_min         -1.222
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         8910
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+3.1403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0772
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7321
_reflns_number_total             8910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06882d2.cif
_cod_data_source_block           2
_cod_database_code               7120701
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.775
_shelx_estimated_absorpt_t_max   0.880
_shelxl_version_number           2013-4
_shelx_res_checksum              39922