Expanding Heteroscorpionates. Facile Synthesis of New Hybrid Scorpionate/Cyclopentadienyl Ligands and Their Lithium and Group 4 Metal Compounds: A Combined Experimental and Density Functional Theory Study
Otero, Antonio; Fernández-Baeza, Juan; Antiñolo, Antonio; Tejeda, Juan; Lara-Sánchez, Agustín; Sánchez-Barba, Luis F.; Sánchez-Molina, Margarita; Rodríguez, Ana M.; Bo, Carles; Urbano-Cuadrado, Manuel; Organometallics 26 (2007) 4310–; doi:10.1021/om7003942

data_4083692
_publ_section_title
;
 Expanding Heteroscorpionates. Facile Synthesis of New Hybrid
 Scorpionate/Cyclopentadienyl Ligands and Their Lithium and Group 4 Metal
 Compounds:&#x00A0; A Combined Experimental and Density Functional Theory
 Study
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4310
_journal_paper_doi               10.1021/om7003942
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C29 H29 Cl3 N4 Zr, 2(C4 H8 O)'
_chemical_formula_sum            'C37 H45 Cl3 N4 O2 Zr'
_chemical_formula_weight         775.34
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.935(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2220(11)
_cell_length_b                   23.628(2)
_cell_length_c                   12.8891(12)
_cell_measurement_temperature    173(2)
_cell_volume                     3654.5(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  '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  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0563
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            20933
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  0.9310
_exptl_absorpt_correction_T_min  0.8329
_exptl_absorpt_correction_type   Semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.430
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         7472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0912P)^2^+8.2268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1530
_refine_ls_wR_factor_ref         0.1716
_reflns_number_gt                5339
_reflns_number_total             7472
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7003942-file002.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        3654.6(6)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4083692