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_4343054
_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_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety         'C27 H35 Cl O2 Zr'
_chemical_formula_sum            'C27 H35 Cl O2 Zr'
_chemical_formula_weight         518.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 112.570(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0556(7)
_cell_length_b                   9.8671(5)
_cell_length_c                   17.9498(9)
_cell_measurement_reflns_used    34290
_cell_measurement_temperature    150
_cell_measurement_theta_max      69.20
_cell_measurement_theta_min      2.67
_cell_volume                     2462.3(2)
_computing_cell_refinement       'SAINT V7.68A(Bruker AXS, 2009)'
_computing_data_collection       'APEX2  (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A(Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL  (Bruker AXS, 2003)'
_computing_publication_material  'UdMX (Maris, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker Microstar'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Helios optics'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45592
_diffrn_reflns_theta_full        69.54
_diffrn_reflns_theta_max         69.54
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    4.808
_exptl_absorpt_correction_T_max  0.6807
_exptl_absorpt_correction_T_min  0.5173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 2008)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.358
_refine_diff_density_min         -1.172
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4565
_refine_ls_number_restraints     354
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0757
_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^)+(0.0967P)^2^+20.1757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2042
_refine_ls_wR_factor_ref         0.2052
_reflns_number_gt                4395
_reflns_number_total             4565
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic5b00634_si_002.cif
_cod_data_source_block           fred36(1)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4343054--4343060.cif.
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4343054