On the temperature dependence of H-<i>U</i>~iso~ in the riding hydrogen model
Lübben, Jens; Volkmann, Christian; Grabowsky, Simon; Edwards, Alison; Morgenroth, Wolfgang; Fabbiani, Francesca P. A.; Sheldrick, George M.; Dittrich, Birger; Acta Crystallographica Section A 70 (2014) 309–316; doi:10.1107/S2053273314010626

data_2310141
_publ_contact_author
;
  Dr. Birger Dittrich
  Universitaet Hamburg
  Institut fuer Anorganische und Angewandte Chemie
  Martin-Luther-King-Platz 6
  20146 Hamburg
  Germany

  Dr. Simon Grabowsky
  The University of Western Australia
  School of Chemistry and Biochemistry, M310
  35 Stirling Highway
  Crawley WA 6009
  Australia
;
_publ_section_title
;
 On the temperature dependence of H-<i>U</i>~iso~ in the riding hydrogen
 model
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section A'
_journal_page_first              309
_journal_page_last               316
_journal_paper_doi               10.1107/S2053273314010626
_journal_volume                  70
_journal_year                    2014
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C7 H11 N1 O4, H2 O'
_chemical_formula_sum            'C7 H13 N O5'
_chemical_formula_weight         191.18
_chemical_name_common            'L-hydroxyproline monohydrate'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     isomor
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0123(2)
_cell_length_b                   9.2556(2)
_cell_length_c                   10.2441(2)
_cell_measurement_reflns_used    'not applicable'
_cell_measurement_temperature    250
_cell_measurement_theta_max      'not applicable'
_cell_measurement_theta_min      'not applicable'
_cell_volume                     949.32(3)
_computing_data_collection       'MAATEL/ANSTO control program'
_computing_data_reduction
'argonne_boxes (Wilkinson et al., 1988) & LaueG (Piltz, 2011)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_diffrn_ambient_temperature      250
_diffrn_measured_fraction_theta_full 0.746
_diffrn_measured_fraction_theta_max 0.746
_diffrn_measurement_details      '10 images, exposure time 42 minutes each'
_diffrn_measurement_device       'Laue image-plate diffractometer'
_diffrn_measurement_device_type  KOALA
_diffrn_measurement_method       Laue
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.85
_diffrn_reflns_av_R_equivalents  0.0978
_diffrn_reflns_av_unetI/netI     0.0867
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            13174
_diffrn_reflns_reduction_process 'LaueG (Piltz, 2011)'
_diffrn_reflns_resolution_max    1.54
_diffrn_reflns_theta_full        70.79
_diffrn_reflns_theta_max         70.89
_diffrn_source                   'nuclear reactor'
_diffrn_source_details           'thermal neutrons, supermirror guides'
_diffrn_source_type
'OPAL reactor, ANSTO, Lucas Heights, Australia'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.0
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             144
_exptl_crystal_size_max          1.8
_exptl_crystal_size_mid          1.4
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.70
_refine_diff_density_min         -0.88
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9945
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         9675
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.0001605
_refine_ls_shift/su_mean         0.0000124
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
 Method = Robust Weighting (Prince, 1982)
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
 A~i~ are:
 1.19 -0.518 0.521
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0502
_reflns_number_gt                967
_reflns_number_total             1307
_reflns_threshold_expression     I>3.0\s(I)
_oxford_refine_ls_scale          0.4243(18)
_cod_data_source_file            kx5033sup1.cf
_cod_data_source_block           hydroxyproline250K
_cod_depositor_comments
'Adding full bibliography for 2310130--2310141.cif.'
_cod_original_formula_sum        'C7 H13 N1 O5'
_cod_database_code               2310141
_iucr_refine_instruction_details_constraints
;
BLOCK 
CONT SCALE 
CONT O    (    1 ,X'S,U'S) UNTIL  H(12) 
CONT H    (   90, X'S, U[ISO]) UNTIL LAST 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;