The XIPHOS diffraction facility for extreme sample conditions
Probert, Michael R.; Robertson, Craig M.; Coome, Jonathan A.; Howard, Judith A. K.; Michell, Brian C.; Goeta, Andrés E.; Journal of Applied Crystallography 43 (2010) 1415–1418; doi:10.1107/S0021889810041282

data_2300303
_publ_section_title
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 The XIPHOS diffraction facility for extreme sample conditions
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_journal_coeditor_code           HX5107
_journal_issue                   6
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first              1415
_journal_page_last               1418
_journal_paper_doi               10.1107/S0021889810041282
_journal_volume                  43
_journal_year                    2010
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C6 H6 N2 O2'
_chemical_formula_sum            'C6 H6 N2 O2'
_chemical_formula_weight         138.13
_chemical_name_systematic        m-nitroaniline
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.7169(4)
_cell_length_b                   6.5215(2)
_cell_length_c                   5.00140(10)
_cell_measurement_reflns_used    3128
_cell_measurement_temperature    2.0
_cell_measurement_theta_max      30.407
_cell_measurement_theta_min      3.308
_cell_volume                     610.48(3)
_computing_cell_refinement       'Bruker SAINT version 7.68a (Bruker, 2010)'
_computing_data_collection       'Bruker APEXII v2010.1-2 (Bruker, 2010)'
_computing_data_reduction        'Bruker SAINT version 7.68a (Bruker, 2010)'
_computing_molecular_graphics
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OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
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_computing_publication_material
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OLEX2: a complete structure solution, refinement and analysis program. 
Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution
;
A short history of SHELX (Sheldrick, 2007)/Bruker
;
_diffrn_ambient_temperature      2.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker APEXII area detector'
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       'XIPHOS four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    focused
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Bruker TXS with Helios Optics'
_diffrn_radiation_type           'MO K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0167
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            9614
_diffrn_reflns_theta_full        30.41
_diffrn_reflns_theta_max         30.41
_diffrn_reflns_theta_min         2.18
_diffrn_source                   'rotating anode'
_diffrn_source_target            Mo
_diffrn_source_type              'Bruker TXS with Helios Optics'
_exptl_absorpt_coefficient_mu    0.116
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.6107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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 SADABS-2008/1 (Bruker,2008) was used for absorption correction.
 R(int) was 0.0670 before and 0.0419 after correction.
 The Ratio of minimum to maximum transmission is 0.818632707775.
 The \l/2 correction factor is Not present
;
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             288
_exptl_crystal_preparation       'crystal was mounted on a graphite fibre'
_exptl_crystal_recrystallization_method 'slow evaporation from EtOH'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'not refined as all light atom structure'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         993
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
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calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.2014P] where P=(Fo^2^+2Fc^2^)/3
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_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0880
_reflns_number_gt                935
_reflns_number_total             993
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            hx5107.cif
_cod_data_source_block           mna_2_K
_cod_database_code               2300303