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_4337654
_publ_section_title
;
 Zirconium(IV) Metallocavitands As Blue-Emitting Materials.
;
_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
'C72 H60 N3 O10 Zr3, C4 H10 O,C3.16 H10 O0.79,Cl'
_chemical_formula_sum            'C79.18 H80 Cl N3 O11.8 Zr3'
_chemical_formula_weight         1571.45
_chemical_name_systematic
; 
 ? 
;
_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                70.543(9)
_cell_angle_beta                 77.670(9)
_cell_angle_gamma                63.506(8)
_cell_formula_units_Z            2
_cell_length_a                   14.372(2)
_cell_length_b                   15.973(2)
_cell_length_c                   19.995(3)
_cell_measurement_reflns_used    8067
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.3
_cell_measurement_theta_min      2.2
_cell_volume                     3862.0(10)
_computing_cell_refinement       'SMART APEX II'
_computing_data_collection       'SMART APEX II (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      150(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0815
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            46937
_diffrn_reflns_theta_full        26.53
_diffrn_reflns_theta_max         26.53
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  0.9617
_exptl_absorpt_correction_T_min  0.9081
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'Pale green'
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1615
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
The heavily disordered solvent molecule (EtOEt) 
was squeezed out of the structure
;
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         15837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1223
_reflns_number_gt                9937
_reflns_number_total             15837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic402602d_si_001.cif
_cod_data_source_block           HI04-15-1n(7)
_cod_original_cell_volume        3861.8(10)
_cod_original_formula_sum        'C79.18 H80 Cl N3 O11.80 Zr3'
_cod_database_code               4337654