Enantiospecific synthesis of a planar chiral fluorenylzirconium ansa-metallocene: synthesis and structures of [1-(9-fluorenyl)- and [1-(1-methyl-9-fluorenyl)-2-(2-indenyl)naphthalene]zirconium dichloride
Baker, Robert W.; Foulkes, Michael A.; Turner, Peter; Journal of the Chemical Society, Dalton Transactions  (2000) 431–; doi:10.1039/a910246i

data_7009312
_publ_contact_author
;
    Dr Robert W Baker
    School of Chemsitry (F11)
    University of Sydney
    Sydney NSW 2006
    Australia
;
_publ_section_title
;
 Enantiospecific synthesis of a planar chiral fluorenylzirconium
 ansa-metallocene: synthesis and structures of [1-(9-fluorenyl)- and
 [1-(1-methyl-9-fluorenyl)-2-(2-indenyl)naphthalene]zirconium
 dichloride
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              431
_journal_paper_doi               10.1039/a910246i
_journal_year                    2000
_chemical_formula_moiety         'C33 H22 Cl2 Zr '
_chemical_formula_sum            'C33 H22 Cl2 Zr'
_chemical_formula_weight         580.66
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_audit_creation_date             1998-05-01
_audit_creation_method           'by teXsan v1.7'
_audit_update_record             ?
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.802(5)
_cell_length_b                   29.313(9)
_cell_length_c                   8.312(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294.2
_cell_measurement_theta_max      18.3
_cell_measurement_theta_min      9.5
_cell_volume                     5068(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'teXsan (MSC, 1995)'
_computing_structure_solution
;
SHELXS86 (Sheldrick, 1985)
;
_diffrn_ambient_temperature      294.2
_diffrn_measurement_device       'Rigaku AFC7R'
_diffrn_measurement_method       \w-\q
_diffrn_orient_matrix_UB_11      -0.04686
_diffrn_orient_matrix_UB_12      0.00743
_diffrn_orient_matrix_UB_13      0.00001
_diffrn_orient_matrix_UB_21      0.01048
_diffrn_orient_matrix_UB_22      0.03317
_diffrn_orient_matrix_UB_23      -0.00270
_diffrn_orient_matrix_UB_31      -0.00029
_diffrn_orient_matrix_UB_32      -0.00071
_diffrn_orient_matrix_UB_33      -0.12025
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.05545
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            2817
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         49.93
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        -29.41
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.738
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.605
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_meas      ?
_exptl_crystal_description       acicular
_exptl_crystal_F_000             2352.00
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.85
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.145
_refine_ls_goodness_of_fit_obs   2.145
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     290
_refine_ls_number_reflns         1072
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_obs          0.0820
_refine_ls_shift/esd_max         0.0379
_refine_ls_shift/esd_mean        0.0096
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00016|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0733
_refine_ls_wR_factor_obs         0.0733
_reflns_number_observed          1072
_reflns_number_total             2724
_reflns_observed_criterion       >2.50\s(I)
_cod_data_source_file            a910246i.txt
_cod_data_source_block           rwb4
_cod_depositor_comments
;
 Correcting the data name order in the GEOM_TORSION loop.

 Antanas Vaitkus,
 2018-08-08

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00016|Fo|^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1/[\s^2^(Fo) + 0.00016|Fo|^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5068(3)
_cod_original_sg_symbol_H-M      'P b c a    '
_cod_original_formula_sum        'C33 H22 Cl2 Zr '
_cod_database_code               7009312