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_4515730
_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 H31 Mn N2 O2 P2'
_chemical_formula_sum            'C39 H31 Mn N2 O2 P2'
_chemical_formula_weight         676.54
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
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_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   37.5012(5)
_cell_length_b                   37.5012(5)
_cell_length_c                   11.98047(16)
_cell_measurement_reflns_used    18784
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      4.5770
_cell_volume                     14591.3(3)
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_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 0.999
_diffrn_measured_fraction_theta_max 0.991
_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  0.0350
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27956
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.372
_diffrn_reflns_theta_min         3.933
_exptl_absorpt_coefficient_mu    4.545
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.989
_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            orange
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       needle
_exptl_crystal_F_000             6300
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         6825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0501
_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^)+(0.1021P)^2^+13.9507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1473
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6162
_reflns_number_total             6825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b02208_si_002.cif
_cod_data_source_block           complex7
_cod_original_cell_volume        14591.4(4)
_cod_database_code               4515730
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.680
_shelx_estimated_absorpt_t_max   0.876
_shelx_res_checksum              42007
_shelx_hkl_checksum              16165