Fusion and Desulfurization Reactions of Thiomorpholinochlorins.
Sharma, Meenakshi; Banerjee, Subhadeep; Zeller, Matthias; Brückner, Christian; The Journal of organic chemistry 81 (2016) 12350–12356; doi:10.1021/acs.joc.6b02383

data_4037452
_publ_section_title
;
 Fusion and Desulfurization Reactions of Thiomorpholinochlorins.
;
_journal_issue                   24
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              12350
_journal_page_last               12356
_journal_paper_doi               10.1021/acs.joc.6b02383
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C46 H30 N4 Ni S, 1.299(C6 H14)'
_chemical_formula_sum            'C53.794 H48.186 N4 Ni S'
_chemical_formula_weight         841.43
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   41.2820(5)
_cell_length_b                   41.2820(5)
_cell_length_c                   14.1626(2)
_cell_measurement_reflns_used    85908
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.199
_cell_measurement_theta_min      5.671
_cell_volume                     20902.3(5)
_computing_cell_refinement       'HKL3000 (Otwinowski & Minor, 1997)'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)'
_computing_data_reduction        'HKL3000 (Otwinowski & Minor, 1997)'
_computing_structure_refinement
;  
SHELXL-2014/7 (Sheldrick, 2014), 
SHELXLE Rev794 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type
'Rigaku Rapid II curved image plate diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            85908
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.199
_diffrn_reflns_theta_min         5.671
_diffrn_source                   'microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    1.317
_exptl_absorpt_correction_T_max  0.760
_exptl_absorpt_correction_T_min  0.622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       block
_exptl_crystal_F_000             7973.1
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.000039(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         9054
_refine_ls_number_restraints     330
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0622
_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^)+(0.0243P)^2^+161.1053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1432
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8763
_reflns_number_total             9054
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b02383_si_004.cif
_cod_data_source_block           MS-A-162
_cod_original_cell_volume        20902.3(6)
_cod_database_code               4037452
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.678
_shelx_estimated_absorpt_t_max   0.760
_shelx_res_checksum              49016
_shelx_hkl_checksum              68573