A Tantalum Methylidene Complex Supported by a Robust and Sterically Encumbering Aryloxide Ligand
Searles, Keith; Pinter, Balazs; Chen, Chun-Hsing; Mindiola, Daniel J.; Organometallics 33 (2014) 4192–; doi:10.1021/om500197k

data_4084184
_publ_section_title
;
 A Tantalum Methylidene Complex Supported by a Robust and Sterically
 Encumbering Aryloxide Ligand
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4192
_journal_paper_doi               10.1021/om500197k
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C97 H97 Cl1 O2 P1 Ta1'
_chemical_formula_sum            'C97 H97 Cl O2 P Ta'
_chemical_formula_weight         1542.21
_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   difmap
_atom_sites_solution_primary     other
_audit_creation_date             13-05-20
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 95.9980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9466(8)
_cell_length_b                   21.6378(10)
_cell_length_c                   19.8521(9)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100
_cell_measurement_theta_max      14
_cell_measurement_theta_min      2
_cell_volume                     8094.1(6)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 83.33
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details      '0.5 degree frames measured for 0.3s each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  'Si 1 1 1 and 3 1 1'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.125
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            23384
_diffrn_reflns_theta_full        12.700
_diffrn_reflns_theta_max         16.933
_diffrn_reflns_theta_min         0.812
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.459
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate fragment'
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.007
_refine_diff_density_max         3.48
_refine_diff_density_min         -4.35
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         23329
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.0035754
_refine_ls_shift/su_mean         0.0000737
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 8.84P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1094
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.1094
_reflns_limit_h_max              26
_reflns_limit_h_min              -26
_reflns_limit_k_max              30
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                14729
_reflns_number_total             14158
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.13
_oxford_diffrn_Wilson_scale      163.03
_oxford_refine_ls_r_factor_ref   0.1085
_oxford_refine_ls_scale          0.082389(10)
_oxford_reflns_number_all        23330
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_structure_analysis_title 'CMC0948_0m in P2(1)/n'
_cod_data_source_file            om500197k_si_002.cif
_cod_data_source_block           13509
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
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.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' 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 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4084182--4084184.cif.
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C97 H97 Cl1 O2 P1 Ta1'
_cod_database_code               4084184