<i>N</i>'-<i>tert</i>-Butyl-4-chloro-<i>N</i>'-(4-oxo-4<i>H</i>-chromen-3-ylcarbonyl)benzohydrazide 0.65-hydrate
Pei-Liang Zhao; Wei Huang; Zhong-Zhen Zhou; Guang-Fu Yang; Acta Crystallographica Section E 61 (2005) o3738–o3740; doi:10.1107/S1600536805033118

data_2207290
_publ_section_title
;<i>N</i>'-<i>tert</i>-Butyl-4-chloro-<i>N</i>'-(4-oxo-4<i>H</i>-chromen-3-ylcarbonyl)benzohydrazide
 0.65-hydrate
;
_journal_coeditor_code           LH6513
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3738
_journal_page_last               o3740
_journal_paper_doi               10.1107/S1600536805033118
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C21 H19 Cl N2 O4 , 0.65H2 O'
_chemical_formula_moiety         'C21 H19 Cl N2 O4 , 0.65H2 O'
_chemical_formula_sum            'C21 H20.3 Cl N2 O4.65'
_chemical_formula_weight         409.23
_chemical_melting_point          496
_chemical_name_systematic
;
N'-tert-Butyl-4-chloro-N'-(4-oxo-4H-chromen-3-ylcarbonyl)benzohydrazide
0.65-hydrate
;
_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_creation_method           SHELXL97
_cell_angle_alpha                75.463(2)
_cell_angle_beta                 81.619(3)
_cell_angle_gamma                77.108(3)
_cell_formula_units_Z            2
_cell_length_a                   6.7913(11)
_cell_length_b                   11.7863(18)
_cell_length_c                   13.799(2)
_cell_measurement_reflns_used    4083
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      27.01
_cell_measurement_theta_min      2.63
_cell_volume                     1037.5(3)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'SHELXTL (Bruker, 2001) and PLATON (Spek, 2003)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7452
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.215
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             427
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.299
_refine_ls_extinction_coef       0.032(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         3610
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.1051P)^2^+0.222P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1699
_refine_ls_wR_factor_ref         0.1816
_reflns_number_gt                2910
_reflns_number_total             3610
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6513.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-03-21
;
_cod_original_formula_sum        'C21 H20.30 Cl N2 O4.65'
_cod_database_code               2207290
_cod_database_fobs_code          2207290