Stoichiometric Reactivity Relevant to the Mor-DalPhos/Pd-Catalyzed Cross-Coupling of Ammonia and 1-Bromo-2-(phenylethynyl)benzene
Alsabeh, Pamela G.; McDonald, Robert; Stradiotto, Mark; Organometallics 31 (2012) 1049–; doi:10.1021/om201122q

data_4068125
_publ_section_title
;
 Stoichiometric Reactivity Relevant to the Mor-DalPhos/Pd-Catalyzed
 Cross-Coupling of Ammonia and 1-Bromo-2-(phenylethynyl)benzene
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              1049
_journal_paper_doi               10.1021/om201122q
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C44 H51 N O P Pd, C4 H10 O, C F3 O3 S'
_chemical_formula_sum            'C49 H61 F3 N O5 P Pd S'
_chemical_formula_weight         970.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.5094(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7231(8)
_cell_length_b                   16.1892(12)
_cell_length_c                   26.826(2)
_cell_measurement_reflns_used    9305
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.04
_cell_measurement_theta_min      2.34
_cell_volume                     4487.4(6)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-2008 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11664
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.70
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  0.9252
_exptl_absorpt_correction_T_min  0.7812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.992
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         11664
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+8.4202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1239
_reflns_number_gt                10624
_reflns_number_total             11664
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om201122q_si_001.cif
_cod_data_source_block           dal1159
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4068125