Synthesis and reactivity of palladium hydrido-solvento complexes, including a key intermediate in the catalytic methoxycarbonylation of ethene to methyl propanoate
Clegg, William; Eastham, Graham R.; Elsegood, Mark R. J.; Heaton, Brian T.; Iggo, Jonathan A.; Tooze, Robert P.; Whyman, Robin; Zacchini, Stefano; Journal of the Chemical Society, Dalton Transactions  (2002) 3300–; doi:10.1039/b202372p

data_7011635
_publ_section_title
;
 Synthesis and reactivity of palladium hydrido-solvento complexes,
 including a key intermediate in the catalytic methoxycarbonylation of
 ethene to methyl propanoate
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3300
_journal_paper_doi               10.1039/b202372p
_journal_year                    2002
_chemical_formula_sum            'C34 H66 O8 P2 Pd S2'
_chemical_formula_weight         835.36
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             1998-04-06
_audit_creation_method           'by teXsan v1.7'
_audit_update_record             ?
_cell_angle_alpha                109.17(4)
_cell_angle_beta                 108.21(7)
_cell_angle_gamma                72.06(6)
_cell_formula_units_Z            2
_cell_length_a                   11.87(2)
_cell_length_b                   15.410(7)
_cell_length_c                   11.168(6)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    153.2
_cell_measurement_theta_max      0.0
_cell_measurement_theta_min      0.0
_cell_volume                     1784(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'teXsan (MSC, 1995)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1993)
;
_diffrn_ambient_temperature      153.2
_diffrn_measurement_device       'Rigaku AFC6S'
_diffrn_orient_matrix_UB_11      -0.04127
_diffrn_orient_matrix_UB_12      0.04128
_diffrn_orient_matrix_UB_13      -0.06144
_diffrn_orient_matrix_UB_21      0.02540
_diffrn_orient_matrix_UB_22      0.05520
_diffrn_orient_matrix_UB_23      0.07005
_diffrn_orient_matrix_UB_31      0.07715
_diffrn_orient_matrix_UB_32      -0.01517
_diffrn_orient_matrix_UB_33      -0.02883
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.01724
_diffrn_reflns_av_sigmaI/netI    0.040
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4940
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        -14.19
_diffrn_standards_interval_count 0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            unknown
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_meas      ?
_exptl_crystal_description       unknown
_exptl_crystal_F_000             884.00
_exptl_crystal_size_max          0.00
_exptl_crystal_size_mid          0.00
_exptl_crystal_size_min          0.00
_refine_diff_density_max         0.64
_refine_diff_density_min         -0.72
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.701
_refine_ls_goodness_of_fit_obs   1.701
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     379
_refine_ls_number_reflns         3721
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_obs          0.0397
_refine_ls_shift/esd_max         0.0001
_refine_ls_shift/esd_mean        0.0111
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00031|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0488
_refine_ls_wR_factor_obs         0.0488
_reflns_number_observed          3721
_reflns_number_total             4668
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            b202372p.txt
_cod_data_source_block           983_0009_for_s._Zacchini
_cod_depositor_comments
;
 Correcting the data name order in the GEOM_TORSION loop.

 Antanas Vaitkus,
 2018-08-08

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) +
0.00031|Fo|^2^]' 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) + 0.00031|Fo|^2^]'.

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

The following automatic conversions were performed:
data name '_geom_bond_atom_site_label_D' replaced with
'_geom_hbond_atom_site_label_D' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_bond_atom_site_label_H' replaced with
'_geom_hbond_atom_site_label_H' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_atom_site_label_a' replaced with
'_geom_hbond_atom_site_label_A' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_bond_distance_DH' replaced with '_geom_hbond_distance_DH'
as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_distance_HA' replaced with
'_geom_hbond_distance_HA' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_distance_DA' replaced with
'_geom_hbond_distance_DA' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_angle_DHA' replaced with '_geom_hbond_angle_DHA' as
specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_contact_site_symmetry_A' replaced with
'_geom_hbond_site_symmetry_A' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 5005 2017-03-03 11:38:54Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1       '
_cod_original_formula_sum        'C34 H66 O8 P2 Pd S2 '
_cod_database_code               7011635