Amino acid-derived N-heterocyclic carbene palladium complexes for aqueous phase Suzuki‒Miyaura couplings
Steeples, Elliot; Kelling, Alexandra; Schilde, Uwe; Esposito, Davide; New J. Chem. 40 (2016) 4922–; doi:10.1039/C5NJ03337C

data_7055437
_publ_section_title
;
 Amino acid-derived N-heterocyclic carbene palladium complexes for aqueous
 phase Suzuki--Miyaura couplings
;
_journal_issue                   6
_journal_name_full               'New J. Chem.'
_journal_page_first              4922
_journal_paper_doi               10.1039/C5NJ03337C
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C22 H32 Cl2 N4 O8 Pd'
_chemical_formula_sum            'C22 H32 Cl2 N4 O8 Pd'
_chemical_formula_weight         657.81
_chemical_name_systematic
'trans-dichlorido-bis(1,3-bis(2-ethoxy-2-oxoethyl)-imidazol-2-ylidine)- palladium(II)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-02-22 deposited with the CCDC.
2016-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.793(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.2261(3)
_cell_length_b                   27.7257(6)
_cell_length_c                   17.0282(4)
_cell_measurement_reflns_used    59489
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      25.21
_cell_measurement_theta_min      1.41
_cell_volume                     5688.1(2)
_computing_cell_refinement       'X-AREA (Stoe, 2011)'
_computing_data_collection       'X-AREA (Stoe, 2011)'
_computing_data_reduction        'X-RED (Stoe, 2009)'
_computing_molecular_graphics    'Diamond (Blankenburg, 2015)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      210(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
; 
 360 frames, 1 min exposure time
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scan, \d \w = 1.0 deg'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            69663
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.626
_diffrn_reflns_theta_max         24.626
_diffrn_reflns_theta_min         1.418
_exptl_absorpt_coefficient_mu    0.890
_exptl_absorpt_correction_T_max  0.9592
_exptl_absorpt_correction_T_min  0.7281
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-RED (Stoe, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pale
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.230
_refine_diff_density_min         -1.225
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.00059(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         9541
_refine_ls_number_restraints     167
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0297
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+3.2999P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                8093
_reflns_number_total             9541
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03337c2.cif
_cod_data_source_block           4a
_cod_depositor_comments
'Adding full bibliography for 7055437--7055440.cif.'
_cod_database_code               7055437
_shelx_res_checksum              49536