Dimethyl hydrazine-1,2-dicarboxylate–triphenylphosphine oxide (1/1)
Doboszewski, Bogdan; McGarrah, James; Nazarenko, Alexander Y.; da Paixao Soares, Fabio; Acta Crystallographica Section E 67 (2011) o1565–; doi:10.1107/S160053681101991X

data_2230803
_publ_section_title
;
 Dimethyl hydrazine-1,2-dicarboxylate--triphenylphosphine oxide (1/1)
;
_journal_coeditor_code           MW2011
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1565
_journal_paper_doi               10.1107/S160053681101991X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C4 H8 N2 O4, C18 H15 O P'
_chemical_formula_moiety         'C4 H8 N2 O4, C18 H15 O P'
_chemical_formula_sum            'C22 H23 N2 O5 P'
_chemical_formula_weight         426.39
_chemical_name_systematic
;
Dimethyl hydrazine-1,2-dicarboxylate--triphenylphosphine oxide (1/1)
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 109.090(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.494(3)
_cell_length_b                   8.5545(9)
_cell_length_c                   20.4426(19)
_cell_measurement_reflns_used    3730
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.42
_cell_measurement_theta_min      2.51
_cell_volume                     4378.4(8)
_computing_cell_refinement       'APEX2 (Bruker, 2010) and SAINT (Bruker, 2009)'
_computing_data_collection       'GIS (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2009) and XPREP (Bruker, 2009)'
_computing_molecular_graphics
;
<i>ORTEP-3 for Windows</i> (Farrugia, 1997) and <i>Mercury</i>
(Macrae  <i>et al.</i>, 2008)
;
_computing_publication_material  '<i>PLATON</i> (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008<i>b</i>)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008<i>b</i>)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART X2S'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'doubly curved silicon crystal'
_diffrn_radiation_source         'XOS X-beam microfocus source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20468
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS (Sheldrick, 2008<i>a</i>)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.297
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         3862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0953
_reflns_number_gt                2956
_reflns_number_total             3862
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            mw2011.cif
_cod_data_source_block           I
_cod_original_cell_volume        4378.3(8)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2230803
_cod_database_fobs_code          2230803