Regioselective Synthesis of Vitamin K3 Based Dihydrobenzophenazine Derivative: Their Novel Crystal Structure and DFT Studies
Chadar, Dattatray; Rao, Soniya S.; Gejji, Shridhar P.; Ugale, Bharat Pandurangrao; Nagaraja, C. M.; Nikalje, Milind D.; Salunke-Gawali, Sunita; RSC Adv.  (2015) –; doi:10.1039/C5RA13169C

data_7221969
_publ_section_title
;
 Regioselective Synthesis of Vitamin K3 Based Dihydrobenzophenazine
 Derivative: Their Novel Crystal Structure and DFT Studies
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA13169C
_journal_year                    2015
_chemical_formula_moiety         'C94 H86 N20 O18 Zn4'
_chemical_formula_sum            'C94 H86 N20 O18 Zn4'
_chemical_formula_weight         2045.31
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc11nr6n
_audit_creation_method           SHELXL-97
_audit_update_record
;
2013-11-22 deposited with the CCDC.
2015-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                81.1120(10)
_cell_angle_beta                 87.7110(10)
_cell_angle_gamma                84.5360(10)
_cell_formula_units_Z            2
_cell_length_a                   10.7575(4)
_cell_length_b                   15.3180(6)
_cell_length_c                   29.3906(13)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.4
_cell_measurement_theta_min      2.2
_cell_volume                     4761.6(3)
_computing_cell_refinement       'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0793
_diffrn_reflns_av_sigmaI/netI    0.0689
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            135441
_diffrn_reflns_theta_full        28.42
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    1.073
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.6669
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2108
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.323
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1242
_refine_ls_number_reflns         23865
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+3.2314P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1337
_reflns_number_gt                15835
_reflns_number_total             23865
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra13169c2.cif
_cod_data_source_block           4bpdh
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7221969