Heteroatom Derivatives of Cyclopentadienylaluminum: X-ray Crystal Structure of (η5-C5H5)(2,6-t-Bu-4-Me-C6H2O)2Al
James D. Fisher; Pamela J. Shapiro; P. M. H. Budzelaar; Richard J. Staples; Inorganic Chemistry 37 (1998) 1295–1298; doi:10.1021/ic970376m

data_4322693
_publ_section_title
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 Heteroatom Derivatives of Cyclopentadienylaluminum: X-ray Crystal
 Structure of (\h5-C5H5)(2,6-t-Bu-4-Me-C6H2O)2Al
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1295
_journal_page_last               1298
_journal_paper_doi               10.1021/ic970376m
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C35 H51 Al O2'
_chemical_formula_weight         530.74
_chemical_name_systematic
;
 ?
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_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 103.0990(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4870(6)
_cell_length_b                   11.5404(5)
_cell_length_c                   18.3294(7)
_cell_measurement_reflns_used    4434
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.2
_cell_volume                     3190.7(2)
_computing_cell_refinement       'SMART (SIEMENS, V4.033, 1994)'
_computing_data_collection       'ASTRO (SIEMENS, V4.033, 1994)'
_computing_data_reduction        'SAINT (SIEMENS, V4.035, 1994)'
_computing_molecular_graphics    'SHELXTL (SIEMENS, 1994, ver 5.04)'
_computing_publication_material  'CIFTAB (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Siemens CCD'
_diffrn_measurement_method       '\w oscillation, 0.3 deg'
_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  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            8229
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 'beginning & end'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.9510
_exptl_absorpt_correction_T_min  0.9086
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.182
_refine_ls_goodness_of_fit_obs   1.233
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3232
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.170
_refine_ls_restrained_S_obs      1.217
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_obs          0.0755
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+8.6524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1599
_refine_ls_wR_factor_obs         0.1489
_reflns_number_observed          2605
_reflns_number_total             3232
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970376m.cif
_cod_data_source_block           pjs46f
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+8.6524P] where P=(Fo^2^+2Fc^2^)/3' 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^2^)+(0.0328P)^2^+8.6524P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4322693