M2+and Ln3±catalyzed synthesis of a [1,2,4]triazine core via intramolecular C–H/N–H functionalization and C–N bond formation (M = Mn, Zn, Cd; Ln = Dy, Tb)
Chen, Wen-Bin; Li, Zhi-Xin; Yu, Xin-Wei; Yang, Meng; Qiu, Yan-Xuan; Dong, Wen; New J. Chem. 39 (2015) 1222–; doi:10.1039/C4NJ01027B

data_7054561
_publ_section_title
;
 M2+and Ln3+-catalyzed synthesis of a [1,2,4]triazine core via
 intramolecular C--H/N--H functionalization and C--N bond formation (M =
 Mn, Zn, Cd; Ln = Dy, Tb)
;
_journal_issue                   2
_journal_name_full               'New J. Chem.'
_journal_page_first              1222
_journal_paper_doi               10.1039/C4NJ01027B
_journal_volume                  39
_journal_year                    2015
_chemical_formula_sum            'C8 H6.5 N5 O1.75'
_chemical_formula_weight         200.68
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-11-19 deposited with the CCDC.
2014-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 123.384(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   26.008(3)
_cell_length_b                   6.8360(8)
_cell_length_c                   22.709(3)
_cell_measurement_reflns_used    5744
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.080
_cell_measurement_theta_min      1.88
_cell_volume                     3371.3(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean none
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15117
_diffrn_reflns_theta_full        27.08
_diffrn_reflns_theta_max         27.08
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_T_max  0.9879
_exptl_absorpt_correction_T_min  0.9666
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.0015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3713
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1531
_reflns_number_gt                2662
_reflns_number_total             3713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4nj01027b2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 7054561--7054565.cif.

2018-03-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C32 H26 N20 O7'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     802.73
_cod_database_code               7054561