Highly efficient desymmetrisation of a tricarbonylchromium 1,4-dibromonaphthalene complex by asymmetric SuzukiMiyaura coupling
Xavier Urbaneja; Audrey Mercier; Celine Besnard; Peter Kundig; Chem.Commun. 47 (2011) 3739–; doi:10.1039/c1cc10347d

data_7106160
_publ_section_title
;
 Highly efficient desymmetrisation of a tricarbonylchromium
 1,4-dibromonaphthalene complex by asymmetric Suzuki&#x0096;Miyaura
 coupling
;
_journal_name_full               Chem.Commun.
_journal_page_first              3739
_journal_paper_doi               10.1039/c1cc10347d
_journal_volume                  47
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C51 H40 N O2 P Pd, 0.5(C7 H14), F6 Sb'
_chemical_formula_sum            'C54.5 H47 F6 N O2 P Pd Sb'
_chemical_formula_weight         1121.09
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.5930(10)
_cell_length_b                   12.5930(10)
_cell_length_c                   59.124(6)
_cell_measurement_reflns_used    49480
_cell_measurement_temperature    170
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      3.6
_cell_volume                     9376.1(14)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'IPDS (Stoe & Cie, 1996)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_limit_l_min       -72
_diffrn_reflns_number            58517
_diffrn_reflns_theta_full        25.831
_diffrn_reflns_theta_max         25.831
_diffrn_reflns_theta_min         3.666
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.061
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             4504
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.73
_refine_diff_density_min         -0.94
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.09(2)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9205
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         8953
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.0151026
_refine_ls_shift/su_mean         0.0002853
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
4.55 5.46 1.88
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0965
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.0965
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              72
_reflns_limit_l_min              0
_reflns_number_gt                8670
_reflns_number_total             8966
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.83
_oxford_diffrn_Wilson_scale      0.24
_oxford_refine_ls_r_factor_ref   0.0458
_oxford_refine_ls_scale          0.067617(9)
_oxford_reflns_number_all        8953
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            c1cc10347d.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

2018-06-18
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C109 H94 F12 N2 O4 P2 Pd2 Sb2'
_cod_original_formula_weight         2242.18
_cod_original_formula_moiety         '2(C51 H40 N O2 P Pd), C7 H14, 2(F6 Sb) '
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 43 21 2 '
_cod_database_code               7106160