Synthesis of Carboxylate Cp*Zr(IV) Species: Toward the Formation of Novel Metallocavitands.
Daigle, Maxime; Bi, Wenhua; Légaré, Marc-André; Morin, Jean-François; Fontaine, Frédéric-Georges; Inorganic chemistry 54 (2015) 5547–5555; doi:10.1021/acs.inorgchem.5b00634

data_4343057
_publ_section_title
;
 Synthesis of Carboxylate Cp*Zr(IV) Species: Toward the Formation of Novel
 Metallocavitands.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5547
_journal_page_last               5555
_journal_paper_doi               10.1021/acs.inorgchem.5b00634
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         '     C48 H52 O10 Zr2, C4 H10 O'
_chemical_formula_sum            'C52 H62 O11 Zr2'
_chemical_formula_weight         1045.46
_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                92.4060(10)
_cell_angle_beta                 90.8950(10)
_cell_angle_gamma                98.2720(10)
_cell_formula_units_Z            2
_cell_length_a                   10.36140(10)
_cell_length_b                   11.85310(10)
_cell_length_c                   20.0032(2)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      2.3
_cell_volume                     2428.40(4)
_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      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX II CCD area detector'
_diffrn_measurement_method       '\w 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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            57250
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  0.9528
_exptl_absorpt_correction_T_min  0.9001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.143
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         9873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+2.3954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                8276
_reflns_number_total             9873
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00634_si_002.cif
_cod_data_source_block           md323_0m(3@200K)
_cod_depositor_comments
'Adding full bibliography for 4343054--4343060.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4343057