X-ray and neutron diffraction studies of the non-linear optical compounds MBANP and MBADNP at 20K: charge-density and hydrogen-bonding analyses
Cole, Jacqueline M.; Goeta, Andrés E.; Howard, Judith A. K.; McIntyre, Garry J.; Acta Crystallographica Section B 58 (2002) 690–700; doi:10.1107/S0108768102006109

data_2103304
_publ_section_title
;
 X-ray and neutron diffraction studies of the non-linear optical
 compounds MBANP and MBADNP at 20K: charge-density and hydrogen-bonding
 analyses
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              690
_journal_page_last               700
_journal_paper_doi               10.1107/S0108768102006109
_journal_volume                  58
_journal_year                    2002
_chemical_formula_sum            'C13 H13 N3 O2'
_chemical_formula_weight         243.00
_chemical_name_common            'methylbenzylaminonitropyridine (MBANP)'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.65(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.3210(10)
_cell_length_b                   6.2930(10)
_cell_length_c                   17.650(4)
_cell_measurement_reflns_used    4
_cell_measurement_temperature    20.00(10)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      10
_cell_volume                     589.8(2)
_computing_cell_refinement       'RAFD9 (local program)'
_computing_data_collection       'MAD (Barthelemy, 1984)'
_computing_data_reduction        'RACER (Wilkinson et al, 1988)'
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1995)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      20.00(10)
_diffrn_measurement_device       'The high-flux four-circle diffractometer, D9'
_diffrn_measurement_method       '\w-x-\q scans'
_diffrn_radiation_monochromator  'Cu (220)'
_diffrn_radiation_probe          neutron
_diffrn_radiation_source
'Institut Laue Langevin Reactor, Grenoble, France'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.83717
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4116
_diffrn_reflns_theta_max         46.46
_diffrn_reflns_theta_min         2.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    0.1582
_exptl_absorpt_correction_T_max  0.8574
_exptl_absorpt_correction_T_min  0.7263
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Gaussian integration (Coppens et al, 1965)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    none
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             182
_exptl_crystal_size_max          4.3
_exptl_crystal_size_mid          2.0
_exptl_crystal_size_min          1.0
_refine_diff_density_max         1.795
_refine_diff_density_min         -1.868
_refine_ls_abs_structure_details
;
Absolute structure known a priori from reagents in synthesis
(see paper)
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.557
_refine_ls_goodness_of_fit_obs   2.632
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         2799
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      2.679
_refine_ls_restrained_S_obs      2.631
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_obs          0.0732
_refine_ls_shift/esd_max         -0.004
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1111
_refine_ls_wR_factor_obs         0.1051
_reflns_number_observed          2619
_reflns_number_total             2805
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            an0602.cif
_cod_data_source_block           MBANP
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               2103304
_cod_database_fobs_code          2103304