Abundant Polymorphism in a System with Multiple Hydrogen-Bonding Opportunities: Oxalyl Dihydrazide
Shinbyoung Ahn; Fang Guo; Benson M. Kariuki; Kenneth D. M. Harris; Journal of the American Chemical Society 128 (2006) 8441–8452; doi:10.1021/ja0573155

data_4110684
_publ_contact_author
;
K.D.M. Harris,
School of Chemistry, 
Cardiff University, Park Place, 
Cardiff CF10 3AT, Wales
;
_publ_contact_author_email       HarrisKDM@cardiff.ac.uk
_publ_section_title
;
 Abundant Polymorphism in a System with Multiple Hydrogen-Bonding
 Opportunities: Oxalyl Dihydrazide
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8441
_journal_page_last               8452
_journal_paper_doi               10.1021/ja0573155
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C2 H6 N4 O2'
_chemical_formula_sum            'C2 H6 N4 O2'
_chemical_formula_weight         118.11
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 119.006(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   3.6608(5)
_cell_length_b                   14.550(2)
_cell_length_c                   5.0646(8)
_cell_measurement_reflns_used    339
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      70.04
_cell_measurement_theta_min      6.08
_cell_volume                     235.93(6)
_computing_cell_refinement       SAINTPLUS
_computing_data_collection       SMART
_computing_data_reduction        SAINTPLUS
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Bruker Smart 6000 CCD'
_diffrn_measurement_method       'CCD scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            1344
_diffrn_reflns_theta_full        70.04
_diffrn_reflns_theta_max         70.04
_diffrn_reflns_theta_min         6.08
_exptl_absorpt_coefficient_mu    1.258
_exptl_absorpt_correction_T_max  0.9712
_exptl_absorpt_correction_T_min  0.7891
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       plate
_exptl_crystal_F_000             124
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.151
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     45
_refine_ls_number_reflns         412
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0492P)^2^+0.0498P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0951
_reflns_number_gt                339
_reflns_number_total             412
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0573155si20051103_024327_4.cif
_cod_data_source_block           delta
_cod_database_code               4110684