Highly active NHC‒Pd(ii) complexes for cross coupling of aryl chlorides and arylboronic acids: an investigation of the effect of remote bulky groups
Han, Fangwai; Xu, Ying; Zhu, Rongjiao; Liu, Guiyan; Chen, Chen; Wang, Jianhui; New Journal of Chemistry 42 (2018) 7422–; doi:10.1039/C8NJ01047A

data_7057253
_publ_section_title
;
 Highly active NHC--Pd(ii) complexes for cross coupling of aryl chlorides
 and arylboronic acids: an investigation of the effect of remote bulky
 groups
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              7422
_journal_paper_doi               10.1039/C8NJ01047A
_journal_volume                  42
_journal_year                    2018
_chemical_formula_sum            'C47.2 H36.8 Cl4 N2.4 Pd0.8'
_chemical_formula_weight         864.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2018-02-25 deposited with the CCDC.
2018-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.4920(10)
_cell_angle_gamma                90
_cell_formula_units_Z            5
_cell_length_a                   9.1629(5)
_cell_length_b                   31.1003(17)
_cell_length_c                   17.7075(9)
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_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.69
_cell_measurement_theta_min      2.28
_cell_volume                     5003.0(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.1059
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       23
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_diffrn_reflns_number            37510
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.272
_diffrn_reflns_theta_min         1.309
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_meas      ?
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.170
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_exptl_transmission_factor_max   0.905
_exptl_transmission_factor_min   0.887
_refine_diff_density_max         2.178
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.59(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         19535
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_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0606
_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^)+(0.0563P)^2^+5.1824P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1467
_reflns_Friedel_coverage         0.965
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                14341
_reflns_number_total             19535
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj01047a2.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/home/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.

'_exptl_crystal_density_meas' value 'NONE' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7057250--7057253.cif.
;
_cod_original_formula_sum        'C47.20 H36.80 Cl4 N2.40 Pd0.80'
_cod_database_code               7057253
_shelx_estimated_absorpt_t_min   0.887
_shelx_estimated_absorpt_t_max   0.905
_shelxl_version_number           2013-2
_shelx_res_checksum              59360