In situ cryocrystallization and solid-state structures of furfural and some derivatives
Seidel, Rüdiger W.; Goddard, Richard; Nöthling, Nils; Lehmann, Christian W.; CrystEngComm 21 (2019) 3295–; doi:10.1039/C9CE00435A

data_7232752
_publ_section_title
;
 In situ cryocrystallization and solid-state structures of furfural and
 some derivatives
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              3295
_journal_paper_doi               10.1039/C9CE00435A
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C5 H7 N O'
_chemical_formula_sum            'C5 H7 N O'
_chemical_formula_weight         97.12
_chemical_melting_point          203
_chemical_name_common            furfurylamine
_chemical_name_systematic        1-(2-furyl)methylamine
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-03-22 deposited with the CCDC.    2019-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                94.479(4)
_cell_angle_beta                 92.173(4)
_cell_angle_gamma                96.464(4)
_cell_formula_units_Z            4
_cell_length_a                   5.8006(13)
_cell_length_b                   7.8838(18)
_cell_length_c                   11.355(3)
_cell_measurement_reflns_used    8059
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.7576
_cell_measurement_theta_min      3.0489
_cell_volume                     513.8(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2018)'
_computing_publication_material  'enCIFer (Allen et al., 2004)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32754
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.240
_diffrn_reflns_theta_min         1.801
_diffrn_source                   'microfocus X-ray tube'
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       cylinder
_exptl_crystal_F_000             208
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.500
_exptl_crystal_size_rad          0.250
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         4869
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0740
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0974P)^2^+0.6587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2381
_refine_ls_wR_factor_ref         0.2524
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3729
_reflns_number_total             4869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00435a3.cif
_cod_data_source_block           10328
_cod_depositor_comments
'Adding full bibliography for 7232751--7232754.cif.'
_cod_database_code               7232752
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.932
_shelx_estimated_absorpt_t_max   0.957
_shelx_res_checksum              82455