2-Pyridyl substituents enhance the activity of palladium-phospha-adamantane catalysts for the methoxycarbonylation of phenylacetylene.
Shuttleworth, Timothy A.; Miles-Hobbs, Alexandra M; Pringle, Paul G.; Sparkes, Hazel A.; Dalton transactions (Cambridge, England : 2003) 46 (2016) 125–137; doi:10.1039/c6dt03983a

data_7041335
_publ_section_title
;
 2-Pyridyl substituents enhance the activity of
 palladium-phospha-adamantane catalysts for the methoxycarbonylation of
 phenylacetylene.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              125
_journal_page_last               137
_journal_paper_doi               10.1039/c6dt03983a
_journal_volume                  46
_journal_year                    2016
_chemical_formula_moiety         'C36 H56 Cl2 N2 O6 P2 Pt Si2'
_chemical_formula_sum            'C36 H56 Cl2 N2 O6 P2 Pt Si2'
_chemical_formula_weight         996.93
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-08-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-05 deposited with the CCDC.
2016-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                79.9244(15)
_cell_angle_beta                 83.9717(15)
_cell_angle_gamma                88.2507(15)
_cell_formula_units_Z            1
_cell_length_a                   8.8531(2)
_cell_length_b                   10.6257(3)
_cell_length_c                   11.9101(3)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.95
_cell_measurement_theta_min      2.31
_cell_volume                     1096.92(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_device_type  'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19978
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.970
_diffrn_reflns_theta_min         1.947
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.490
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0518 before and 0.0293 after correction.
The Ratio of minimum to maximum transmission is 0.8133.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       block
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.360
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         5264
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0177
_refine_ls_R_factor_gt           0.0176
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+0.6616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0447
_refine_ls_wR_factor_ref         0.0447
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5263
_reflns_number_total             5264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03983a2.cif
_cod_data_source_block           meso_1g
_cod_depositor_comments
'Adding full bibliography for 7041331--7041344.cif.'
_cod_database_code               7041335
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1-C1 \\sim O1-C2 \\sim O1A-C1 \\sim O1A-C6 \\sim O3A-C4 \\sim O3A-C2 \\sim
O3-C4 \\sim O3-C6
 with sigma of 0.01
 C5A-C1 \\sim C5A-C2 \\sim C5-C1 \\sim C6-C5 \\sim C3-C4 \\sim C2-C3 \\sim
C3A-C4 \\sim C6-C3A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C3A) = Uanis(O3)
Uanis(C3) = Uanis(O3A)
Uanis(C5) = Uanis(O1A)
Uanis(C5A) = Uanis(O1)
4. Others
 Fixed Sof: O3A(0.36543) O1A(0.36543) C3A(0.36543) H3AA(0.36543) H3AB(0.36543)
 C5A(0.36543) H5AA(0.36543) H5AB(0.36543) C5(0.63457) H5A(0.63457) H5B(0.63457)
 O1(0.63457) O3(0.63457) C3(0.63457) H3A(0.63457) H3B(0.63457)
5.a Secondary CH2 refined with riding coordinates:
 C3A(H3AA,H3AB), C5A(H5AA,H5AB), C5(H5A,H5B), C3(H3A,H3B)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C15(H15)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              76135
_olex2_submission_special_instructions 'No special instructions were received'