A heterotrimetallic Pd-Sm-Pd complex for asymmetric Friedel-Crafts alkylations of pyrroles with nitroalkenes.
Zhang, Guoqi; Organic & biomolecular chemistry 10 (2012) 2534–2536; doi:10.1039/c2ob25074h

data_7152289
_publ_section_title
;
 A heterotrimetallic Pd-Sm-Pd complex for asymmetric Friedel-Crafts
 alkylations of pyrroles with nitroalkenes.
;
_journal_issue                   13
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2534
_journal_page_last               2536
_journal_paper_doi               10.1039/c2ob25074h
_journal_volume                  10
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety
;
2(C48 H66 N4 O9 Pd2 Sm), 6(C F3 O3 S), 3(C H4 O), 4(H2 O)
;
_chemical_formula_sum            'C105 H152 F18 N8 O43 Pd4 S6 Sm2'
_chemical_formula_weight         3467.09
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             08-08-25
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.4805(4)
_cell_length_b                   20.3239(6)
_cell_length_c                   24.9820(7)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    203
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     6844.5(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      203
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            173829
_diffrn_reflns_theta_full        32.564
_diffrn_reflns_theta_max         32.564
_diffrn_reflns_theta_min         1.988
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.555
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_description       plate
_exptl_crystal_F_000             3480
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.04
_refine_diff_density_max         8.65
_refine_diff_density_min         -4.44
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.001(11)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     947
_refine_ls_number_reflns         13722
_refine_ls_number_restraints     1749
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.010417
_refine_ls_structure_factor_coef F
_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:
2.07 -0.163 1.62
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0739
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0549
_reflns_limit_h_max              20
_reflns_limit_h_min              -20
_reflns_limit_k_max              30
_reflns_limit_k_min              0
_reflns_limit_l_max              37
_reflns_limit_l_min              0
_reflns_number_gt                13722
_reflns_number_total             24796
_reflns_threshold_expression     I>3.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.17897(18)
_oxford_structure_analysis_title 'gq15_203k_0m in P2(1)2(1)2(1)'
_cod_data_source_file            c2ob25074h.txt
_cod_data_source_block           gq15_203k
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               7152289