Palladium complexes of N-heterocyclic carbenes displaying an unsymmetrical N-alkylfluorenyl/N'-aryl substitution pattern and their behaviour in Suzuki-Miyaura cross coupling.
Almallah, Hamzé; Brenner, Eric; Matt, Dominique; Harrowfield, Jack; Jahjah, Mohamad; Hijazi, Akram; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14516–14529; doi:10.1039/c9dt02948f

data_7701185
_publ_section_title
;
 Palladium complexes of N-heterocyclic carbenes displaying an
 unsymmetrical N-alkylfluorenyl/N'-aryl substitution pattern and their
 behaviour in Suzuki-Miyaura cross coupling.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14516
_journal_page_last               14529
_journal_paper_doi               10.1039/c9dt02948f
_journal_volume                  48
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H31 Cl2 N3 Pd'
_chemical_formula_sum            'C32 H31 Cl2 N3 Pd'
_chemical_formula_weight         634.90
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc21pw7w
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2019-02-18 deposited with the CCDC.    2019-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7007(4)
_cell_length_b                   14.7879(7)
_cell_length_c                   17.9151(7)
_cell_measurement_reflns_used    9315
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.12
_cell_measurement_theta_min      2.22
_cell_volume                     2834.9(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            65424
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.196
_diffrn_reflns_theta_min         1.786
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       prism
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.250
_refine_diff_density_max         1.317
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 3476 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.023(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         8375
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0098P)^2^+3.8829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0703
_reflns_Friedel_coverage         0.798
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                7970
_reflns_number_total             8375
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02948f2.cif
_cod_data_source_block           dmah170920
_cod_depositor_comments
'Adding full bibliography for 7701184--7701187.cif.'
_cod_database_code               7701185
_shelx_estimated_absorpt_t_min   0.722
_shelx_estimated_absorpt_t_max   0.812
_shelxl_version_number           2013-4
_shelx_res_checksum              92264