Zirconium(IV) Metallocavitands As Blue-Emitting Materials.
Iden, Hassan; Bi, Wenhua; Morin, Jean-François; Fontaine, Frédéric-Georges; Inorganic chemistry 53 (2014) 2883–2891; doi:10.1021/ic402602d

data_4337655
_publ_section_title
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 Zirconium(IV) Metallocavitands As Blue-Emitting Materials.
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_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2883
_journal_page_last               2891
_journal_paper_doi               10.1021/ic402602d
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         '4(C72 H54 N3 O10 Zr3), 6(C3 H6 O),'
_chemical_formula_sum            'C313.8 H273 Cl4 N12 O48.6 Zr12'
_chemical_formula_weight         6226.08
_space_group_IT_number           2
_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
_cell_angle_alpha                101.6970(10)
_cell_angle_beta                 115.7730(10)
_cell_angle_gamma                96.6300(10)
_cell_formula_units_Z            1
_cell_length_a                   19.5237(3)
_cell_length_b                   20.4786(3)
_cell_length_c                   21.8854(3)
_cell_measurement_reflns_used    9688
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.2
_cell_measurement_theta_min      2.3
_cell_volume                     7507.6(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT+ (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2007)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            150764
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3177
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_platon_squeeze_details          'The disordered Acetone was squeezed out'
_refine_diff_density_max         1.919
_refine_diff_density_min         -1.370
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1764
_refine_ls_number_reflns         30777
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0732P)^2^+4.0797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1353
_reflns_number_gt                23539
_reflns_number_total             30777
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402602d_si_001.cif
_cod_data_source_block           HI3691(8)
_cod_original_cell_volume        7507.60(19)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C313.80 H273 Cl4 N12 O48.60 Zr12'
_cod_database_code               4337655