An intermolecular pyrene excimer in the pyrene-labeled N-thiophosphorylated thiourea and its nickel(ii) complex
Safin, Damir A.; Babashkina, Maria G.; Mitoraj, Mariusz P.; Kubisiak, Piotr; Robeyns, Koen; Bolte, Michael; Garcia, Yann; Inorganic Chemistry Frontiers 3 (2016) 1419–; doi:10.1039/C6QI00298F

data_4349530
_publ_section_title
;
 An intermolecular pyrene excimer in the pyrene-labeled
 N-thiophosphorylated thiourea and its nickel(ii) complex
;
_journal_issue                   11
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1419
_journal_paper_doi               10.1039/C6QI00298F
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety         'C46 H48 N4 Ni O4 P2 S4'
_chemical_formula_sum            'C46 H48 N4 Ni O4 P2 S4'
_chemical_formula_weight         969.77
_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_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-97
_audit_update_record
;
2016-02-12 deposited with the CCDC.
2016-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.022(5)
_cell_angle_beta                 108.105(5)
_cell_angle_gamma                105.302(5)
_cell_formula_units_Z            1
_cell_length_a                   10.2046(6)
_cell_length_b                   10.7201(7)
_cell_length_c                   10.8463(5)
_cell_measurement_reflns_used    5520
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.5716
_cell_measurement_theta_min      1.8986
_cell_volume                     1083.39(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection       'SNBL Pilatus control'
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.801
_diffrn_measured_fraction_theta_max 0.615
_diffrn_measurement_device_type  'pilatus 2M'
_diffrn_measurement_method       '359 images, \D\F 1.0\% '
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68239
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9801
_diffrn_reflns_theta_full        24.26
_diffrn_reflns_theta_max         31.65
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             506
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         5086
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.6082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0840
_reflns_number_gt                4649
_reflns_number_total             5086
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00298f2.cif
_cod_data_source_block           NiL2
_cod_original_cell_volume        1083.40(11)
_cod_database_code               4349530