Synthesis of Pyrazines and Quinoxalines via Acceptorless Dehydrogenative Coupling Routes Catalyzed by Manganese Pincer Complexes.
Daw, Prosenjit; Kumar, Amit; Espinosa-Jalapa, Noel Angel; Diskin-Posner, Yael; Ben-David, Yehoshoa; Milstein, David; ACS catalysis 8 (2018) 7734–7741; doi:10.1021/acscatal.8b02208

data_4515728
_publ_section_title
;
 Synthesis of Pyrazines and Quinoxalines via Acceptorless Dehydrogenative
 Coupling Routes Catalyzed by Manganese Pincer Complexes.
;
_journal_issue                   9
_journal_name_full               'ACS catalysis'
_journal_page_first              7734
_journal_page_last               7741
_journal_paper_doi               10.1021/acscatal.8b02208
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C39 H27 Br Mn N O2 P2, 2(C4 H8 O)'
_chemical_formula_sum            'C47 H43 Br Mn N O4 P2'
_chemical_formula_weight         882.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                94.2850(10)
_cell_angle_beta                 102.738(2)
_cell_angle_gamma                90.704(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0659(3)
_cell_length_b                   12.6901(2)
_cell_length_c                   13.3087(3)
_cell_measurement_reflns_used    15771
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.6860
_cell_measurement_theta_min      4.4810
_cell_volume                     1981.22(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.22a (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32011
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.503
_diffrn_reflns_theta_min         4.483
_exptl_absorpt_coefficient_mu    5.027
_exptl_absorpt_correction_T_max  0.807
_exptl_absorpt_correction_T_min  0.166
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.22a (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_description       plate
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.016
_refine_diff_density_max         1.338
_refine_diff_density_min         -1.438
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         8038
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+3.4845P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7414
_reflns_number_total             8038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b02208_si_002.cif
_cod_data_source_block           complex1
_cod_database_code               4515728
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.396
_shelx_estimated_absorpt_t_max   0.924
_shelx_res_checksum              89401
_shelx_hkl_checksum              11465