Room temperature, solventless telomerization of isoprene with alcohols using (N-heterocyclic carbene)‒palladium catalysts
Maluenda, Irene; Chen, Ming-Tsz; Guest, Daniel; Mark Roe, S.; Turner, Michael L.; Navarro, Oscar; Catal. Sci. Technol. 5 (2015) 1447–; doi:10.1039/C5CY00058K

data_1518675
_publ_section_title
;
 Room temperature, solventless telomerization of isoprene with alcohols
 using (N-heterocyclic carbene)--palladium catalysts
;
_journal_issue                   3
_journal_name_full               'Catal. Sci. Technol.'
_journal_page_first              1447
_journal_paper_doi               10.1039/C5CY00058K
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         'C27 H39 Cl2 N3 Pd'
_chemical_formula_sum            'C27 H39 Cl2 N3 Pd'
_chemical_formula_weight         582.91
_chemical_name_systematic        (IMes)PdCl2(TEA)
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-10-07
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2014-12-15 deposited with the CCDC.
2015-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.789(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   35.0018(17)
_cell_length_b                   11.2158(5)
_cell_length_c                   15.2054(10)
_cell_measurement_reflns_used    15152
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_cell_volume                     5542.8(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19002
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.040
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear-SM Expert 3.1 b25 (Rigaku, 20112)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_description       shard
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.901
_refine_diff_density_min         -1.160
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         6344
_refine_ls_number_restraints     267
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0351P)^2^+14.0321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1121
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4556
_reflns_number_total             6344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cy00058k2.cif
_cod_data_source_block           2014ncs0275
_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 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 1518674--1518675.cif.
;
_cod_database_code               1518675
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   1.000
_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 body (RIGU) restrains
 Pd1, Cl1, Cl2, N3, C22, C1B, C1C, C20, N8, N9, C18, H1BA, H1BB, C2, H1CA,
 H1CB, C1D, H20A, H20B, C14, C1E, C19, C1F, H18A, H18B, H18C, H2A, H2B, H2C,
 H1DA, H1DB, H1DC, C9, C10, H1E, C12, C16, H1F, C7, C15, C8, C17, C11, C13, C5,
 C1A, C6, H7, H15A, H15B, H15C, H8, H17A, H17B, H17C, H11A, H11B, H11C, C3, H13,
  H5, H1AA, H1AB, H1AC, C4, C1, H4A, H4B, H4C, H1A, H1B, H1C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C1B(H1BA,H1BB), C1C(H1CA,H1CB), C20(H20A,H20B)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7), C8(H8), C13(H13), C1E(H1E), C1F(H1F)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C11(H11A,H11B,H11C),
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C1A(H1AA,H1AB,
 H1AC), C1D(H1DA,H1DB,H1DC)
;
_olex2_submission_special_instructions 'No special instructions were received'