Optimizing the accuracy and precision of the single-pulse Laue technique for synchrotron photo-crystallography
Kamiński, Radosław; Graber, Timothy; Benedict, Jason B.; Henning, Robert; Chen, Yu-Sheng; Scheins, Stephan; Messerschmidt, Marc; Coppens, Philip; Journal of Synchrotron Radiation 17 (2010) 479–485; doi:10.1107/S0909049510019710

data_1513253
_publ_section_title
;
 Optimizing the accuracy and precision of the single-pulse Laue technique
 for synchrotron photo-crystallography
;
_journal_issue                   4
_journal_name_full               'Journal of Synchrotron Radiation'
_journal_page_first              479
_journal_page_last               485
_journal_paper_doi               10.1107/S0909049510019710
_journal_volume                  17
_journal_year                    2010
_chemical_formula_moiety         'C20 H44 Cu4 I4 N4'
_chemical_formula_sum            'C20 H44 Cu4 I4 N4'
_chemical_formula_weight         1102.39
_chemical_melting_point          ?
_chemical_name_systematic
; 
 tetrakis((\m~3~-iodo)-piperidine copper(I))
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.6049(12)
_cell_length_b                   14.6049(12)
_cell_length_c                   7.5464(12)
_cell_measurement_reflns_used    7987
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      30.2991
_cell_measurement_theta_min      2.7893
_cell_volume                     1609.7(3)
_computing_cell_refinement
;
 Cell determination and refinement perfomed with APEX2
 APEX2 (ver. v200911-0), Bruker AXS (2009)
;
_computing_data_collection
;
 Data collection monitored with APEX2
 APEX2 (ver. v2009.11-0), Bruker AXS (2009)
;
_computing_data_reduction
;
 Integration performed with SAINT
 SAINT (ver. V7.68A), Bruker AXS (2009)
;
_computing_structure_refinement
;
 Refined with SHELXL-97
 Sheldrick, G. M.: (2008) Acta Cryst. A64, 112-122
;
_computing_structure_solution
;
 Solved with SHELXS-97
 Sheldrick, G. M.: (2008) Acta Cryst. A64, 112-122
;
_diffrn_ambient_temperature      90(2)
_diffrn_detector                 'APEXII CCD camera'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_orient_matrix_type       'x-axis to radiation source'
_diffrn_orient_matrix_UB_11      0.370597E-1
_diffrn_orient_matrix_UB_12      -0.516555E-1
_diffrn_orient_matrix_UB_13      0.492063E-1
_diffrn_orient_matrix_UB_21      -0.158047E-1
_diffrn_orient_matrix_UB_22      0.199477E-1
_diffrn_orient_matrix_UB_23      0.12302
_diffrn_orient_matrix_UB_31      -0.553619E-1
_diffrn_orient_matrix_UB_32      -0.402733E-1
_diffrn_orient_matrix_UB_33      -0.218059E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            33915
_diffrn_reflns_reduction_process
;
 Scaled and merged with SORTAV
 Blessing, R. H.: (1987) Cryst. Rev. 1, 3-58
 Blessing, R. H.: (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         3.34
_diffrn_source                   'rotating anode X-ray source'
_exptl_absorpt_coefficient_mu    6.458
_exptl_absorpt_correction_T_max  1.155
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Absorption correction done by SORTAV
 Blessing, R. H.: (1995) Acta Cryst. A51, 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.595
_refine_diff_density_min         -1.506
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         2460
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 calc w=1/[\s^2^(Fo^2^)+(0.0105P)^2^+1.0213P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0549
_refine_ls_wR_factor_ref         0.0602
_reflns_number_gt                2056
_reflns_number_total             2460
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            kv5081sup1.cif
_cod_data_source_block           Cu4I4pip4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_diffrn_radiation_probe' value
'X-ray' changed to 'x-ray' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               1513253