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_4110681
_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                 99.298(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   3.6221(4)
_cell_length_b                   6.8322(7)
_cell_length_c                   9.1294(10)
_cell_measurement_reflns_used    394
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      69.83
_cell_measurement_theta_min      8.14
_cell_volume                     222.96(4)
_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 0.969
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker Smart 6000 CCD'
_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  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1340
_diffrn_reflns_theta_full        69.83
_diffrn_reflns_theta_max         69.83
_diffrn_reflns_theta_min         8.14
_exptl_absorpt_coefficient_mu    1.331
_exptl_absorpt_correction_T_max  0.9487
_exptl_absorpt_correction_T_min  0.7767
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.759
_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          0.04
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.140
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       0.031(7)
_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   1.152
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0509P)^2^+0.0520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0903
_reflns_number_gt                394
_reflns_number_total             414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0573155si20051103_024327_1.cif
_cod_data_source_block           alpha
_cod_database_code               4110681