A mechanistic study of allene carboxylation with CO2resulting in the development of a Pd(ii) pincer complex for the catalytic hydroboration of CO2
Suh, Hee-Won; Guard, Louise M.; Hazari, Nilay; Chemical Science 5 (2014) 3859–; doi:10.1039/C4SC01110D

data_1516333
_publ_section_title
;
 A mechanistic study of allene carboxylation with CO2resulting in the
 development of a Pd(ii) pincer complex for the catalytic hydroboration of
 CO2
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              3859
_journal_paper_doi               10.1039/C4SC01110D
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         'C38.73 H59.32 Cl0.14 P2 Pd Si'
_chemical_formula_sum            'C39 H60 P2 Pd Si'
_chemical_formula_weight         725.30
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2014-05-13
_audit_creation_method
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Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
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_cell_angle_alpha                90
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_cell_formula_units_Z            4
_cell_length_a                   12.9946(4)
_cell_length_b                   14.2318(4)
_cell_length_c                   20.8681(15)
_cell_measurement_reflns_used    56378
_cell_measurement_temperature    223
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3798.4(3)
_computing_cell_refinement
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CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
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_computing_data_collection
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CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
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CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      223
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device
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SCXMini: Fixed Chi 2 circle
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_diffrn_measurement_device_type  'Rigaku Mercury2 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Unknown
_diffrn_orient_matrix_type       FS_PROCESS
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_diffrn_orient_matrix_UB_12      0.007285
_diffrn_orient_matrix_UB_13      0.015262
_diffrn_orient_matrix_UB_21      -0.002319
_diffrn_orient_matrix_UB_22      0.062780
_diffrn_orient_matrix_UB_23      -0.021730
_diffrn_orient_matrix_UB_31      -0.013522
_diffrn_orient_matrix_UB_32      0.030704
_diffrn_orient_matrix_UB_33      0.040809
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
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_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         3.030
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       Block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.209
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         8675
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+2.6381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0827
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7534
_reflns_number_total             8675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc01110d2.cif
_cod_data_source_block           007140
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 1516327--1516333.cif.
;
_cod_database_code               1516333
_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. Rigid bond restraints
 C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(Cl1)=1-FVAR(1)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C1)=Sof(H1A)=Sof(H1B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C3(H3), C9(H9), C34(H34), C28(H28)
5.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C4(H4A,H4B), C33(H33A,H33B), C14(H14A,H14B), C10(H10A,H10B),
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C8(H8A,H8B), C11(H11A,H11B),
 C5(H5A,H5B), C35(H35A,H35B), C7(H7A,H7B), C6(H6A,H6B), C39(H39A,H39B),
 C12(H12A,H12B), C13(H13A,H13B), C36(H36A,H36B), C38(H38A,H38B), C37(H37A,H37B),
  C1(H1A,H1B)
5.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C16(H16), C26(H26), C19(H19), C25(H25), C17(H17), C24(H24), C18(H18)
5.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              72620
_shelx_hkl_checksum              53832