Dynamics of water molecules and sodium ions in solid hydrates of nucleotides
Dračínský, Martin; Šála, Michal; Hodgkinson, Paul; CrystEngComm 16 (2014) 6756–; doi:10.1039/c4ce00727a

data_7216245
_publ_section_title
;
 Dynamics of water molecules and sodium ions in solid hydrates of
 nucleotides
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              6756
_journal_paper_doi               10.1039/c4ce00727a
_journal_volume                  16
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C10 H12 N5 O8 P, 2(Na), 7(H2 O)'
_chemical_formula_sum            'C10 H26 N5 Na2 O15 P'
_chemical_formula_weight         533.31
_chemical_name_systematic
;
disodium guanosine-5-phosphate heptahydrate 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-02-06
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.01.22 svn.r2872 for OlexSys, GUI svn.r4747)
;
_audit_update_record
;
2014-02-19 # Formatted by publCIF

;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.0139(3)
_cell_length_b                   21.2524(8)
_cell_length_c                   22.2753(8)
_cell_measurement_reflns_used    3472
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      32.4240
_cell_measurement_theta_min      2.6140
_cell_volume                     4267.2(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.8 (release 13-04-2012 CrysAlis171 .NET)
(compiled Apr 13 2012,18:42:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.8 (release 13-04-2012 CrysAlis171 .NET)
(compiled Apr 13 2012,18:42:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.8 (release 13-04-2012 CrysAlis171 .NET)
(compiled Apr 13 2012,18:42:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0(2)
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0157344000
_diffrn_orient_matrix_UB_12      0.0265512000
_diffrn_orient_matrix_UB_13      0.0182158000
_diffrn_orient_matrix_UB_21      0.0401155000
_diffrn_orient_matrix_UB_22      -0.0138544000
_diffrn_orient_matrix_UB_23      0.0240145000
_diffrn_orient_matrix_UB_31      0.0658340000
_diffrn_orient_matrix_UB_32      0.0147580000
_diffrn_orient_matrix_UB_33      -0.0102413000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1005
_diffrn_reflns_av_unetI/netI     0.1267
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            26750
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         2.62
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.986
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.8 (release 13-04-2012 CrysAlis171 .NET)
(compiled Apr 13 2012,18:42:44)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dull light colourless'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.229
_exptl_crystal_size_min          0.0549
_refine_diff_density_max         1.128
_refine_diff_density_min         -0.984
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         9320
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.427
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0794
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1792
_refine_ls_wR_factor_ref         0.2118
_reflns_number_gt                6470
_reflns_number_total             9320
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00727a4.cif
_cod_data_source_block           GMP
_cod_depositor_comments          'Adding full bibliography for 7216245.cif.'
_cod_database_code               7216245
_chemical_oxdiff_formula         C10H27N4Na2O16P1
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O11W-H11A = O11W-H11B = O12W-H12B
 0.85 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(O25) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.05
4. Others
 Fixed Uiso: H5A(0.03)
5.a Riding coordinates:
 N5(H5A,H5B), N44(H44A,H44B), O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB),
 O4W(H4WA,H4WB), O5W(H5WA,H5WB), O6W(H6WA,H6WB), O7W(H7WA,H7WB), O8W(H8WA,H8WB),
  O9W(H9WA,H9WB), O10W(H10C,H10D), O11W(H11A,H11B), O12W(H12A,H12B), O13W(H13A,
 H13B), O14W(H14A,H14B)
5.b Ternary CH refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C26(H26), C27(H27), C28(H28), C29(H29)
5.c Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C30(H30A,H30B)
5.d Aromatic/amide H refined with riding coordinates:
 C1(H1), N38(H38), C21(H21)
5.e Idealised tetrahedral OH refined as rotating group:
 O4(H4), O23(H23), O24(H24)
;