The First Complexes with Two Metallacycles Fused Around a Common Aryl Substituent: “Akimbo” Complexes
Chicote, María-Teresa; Vicente-Hernández, Inmaculada; Jones, Peter G.; Vicente, José; Organometallics 31 (2012) 6252–; doi:10.1021/om300545k

data_4079175
_publ_section_title
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 The First Complexes with Two Metallacycles Fused Around a Common Aryl
 Substituent: &#x201C;Akimbo&#x201D; Complexes
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_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              6252
_journal_paper_doi               10.1021/om300545k
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C52 H55.72 F3 N5 O5.36 Pd2 S'
_chemical_formula_weight         1138.36
_chemical_name_systematic
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 ? 
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_space_group_IT_number           2
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 89.530(4)
_cell_angle_gamma                86.773(4)
_cell_formula_units_Z            2
_cell_length_a                   10.8315(5)
_cell_length_b                   11.6081(5)
_cell_length_c                   19.9343(8)
_cell_measurement_reflns_used    49517
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.6794
_cell_measurement_theta_min      3.8364
_cell_volume                     2485.68(19)
_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
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_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, Atlas, Nova'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0155
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            66629
_diffrn_reflns_theta_full        75.00
_diffrn_reflns_theta_max         75.87
_diffrn_reflns_theta_min         3.84
_exptl_absorpt_coefficient_mu    6.764
_exptl_absorpt_correction_T_max  0.687
_exptl_absorpt_correction_T_min  0.244
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CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1161
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         6.216
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_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment
'ordered methyls as rigid groups, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         10316
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+11.7819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1216
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                9773
_reflns_number_total             10316
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300545k_si_001.cif
_cod_data_source_block           ooph_faces
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_original_cell_volume        2485.67(19)
_cod_database_code               4079175