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_1517546
_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         'C44 H71 Al O2 P2 Pd Si'
_chemical_formula_sum            'C44 H71 Al O2 P2 Pd Si'
_chemical_formula_weight         855.41
_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             2014-02-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.17 svn.r2891 for OlexSys, GUI svn.r4773)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.726(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.632(3)
_cell_length_b                   23.5987(7)
_cell_length_c                   19.2983(14)
_cell_measurement_reflns_used    67582
_cell_measurement_temperature    93
_cell_measurement_theta_max      24.7
_cell_measurement_theta_min      3.1
_cell_volume                     4660.7(14)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      93
_diffrn_detector                 RX
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device
;
Crystal Goniometer
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_diffrn_measurement_device_type
;
Rigaku RAXIS conversion
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Loop
_diffrn_orient_matrix_type       FS_PROCESS
_diffrn_orient_matrix_UB_11      0.000564
_diffrn_orient_matrix_UB_12      -0.009468
_diffrn_orient_matrix_UB_13      -0.049907
_diffrn_orient_matrix_UB_21      0.010181
_diffrn_orient_matrix_UB_22      0.041086
_diffrn_orient_matrix_UB_23      -0.002838
_diffrn_orient_matrix_UB_31      0.097415
_diffrn_orient_matrix_UB_32      -0.004239
_diffrn_orient_matrix_UB_33      0.083954
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1205
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 0.937
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            127755
_diffrn_reflns_point_group_measured_fraction_full 0.937
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.689
_diffrn_reflns_theta_min         3.054
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.406
_refine_diff_density_min         -1.254
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       0.0076(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         7904
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0902
_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^)+(0.1890P)^2^+18.6753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2489
_refine_ls_wR_factor_ref         0.2734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5919
_reflns_number_total             7904
_reflns_threshold_expression     'I > 2\s(I)'
_cod_duplicate_entry             1516331
_cod_data_source_file            c4sc01110d2.cif
_cod_data_source_block           s14022
_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/current/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 
;
_cod_original_cell_volume        4660.9(16)
_cod_database_code               1517546
_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
 C39-C40
 1.7 with sigma of 0.01
 C39-C40 \\sim C44-C43 \\sim C42-C41
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C40 \\sim C39 \\sim C42 \\sim C41 \\sim C43 \\sim C44: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(C40) = Uanis(C39)
4. Rigid body (RIGU) restrains
 C40, C39, C42, C41, C43, C44
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C7(H7), C26(H26), C32(H32), C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C27(H27A,H27B), C12(H12A,H12B), C37(H37A,H37B), C36(H36A,
 H36B), C28(H28A,H28B), C8(H8A,H8B), C10(H10A,H10B), C2(H2A,H2B), C33(H33A,
 H33B), C9(H9A,H9B), C6(H6A,H6B), C30(H30A,H30B), C3(H3A,H3B), C35(H35A,H35B),
 C31(H31A,H31B), C39(H39A,H39B), C29(H29A,H29B), C34(H34A,H34B), C43(H43A,H43B),
  C41(H41A,H41B), C5(H5A,H5B), C4(H4A,H4B)
5.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C21(H21), C15(H15), C17(H17), C22(H22), C24(H24), C23(H23),
 C16(H16), C38(H38)
5.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C44(H44A,H44B,H44C), C42(H42A,H42B,H42C), C40(H40A,H40B,
 H40C)
;
_shelx_res_checksum              44241
_shelx_hkl_checksum              73175