Insight into a direct solid‒solid transformation: a potential approach for the removal of residual solvents
Yang, Pengpeng; Lin, Chenguang; Zhuang, Wei; Wen, Qingshi; Zou, Fengxia; Zhou, Jingwei; Wu, Jinglan; Ying, Hanjie; CrystEngComm 18 (2016) 1699–; doi:10.1039/C6CE00034G

data_7223962
_publ_section_title
;
 Insight into a direct solid--solid transformation: a potential approach
 for the removal of residual solvents
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1699
_journal_paper_doi               10.1039/C6CE00034G
_journal_volume                  18
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_compound_source        Biotogether
_chemical_formula_moiety         'C10H11N5O6PNa (5 H2O)'
_chemical_formula_sum            'C10 H21 N5 Na O11 P'
_chemical_formula_weight         441.28
_chemical_name_common
'cAMPNa ;  CYCLIC AMP SODIUM SALT;3',5'-CYCLIC AMP SODIUM SALT'
_chemical_name_systematic        'ADENOSINE-3',5'-CYCLIC PHOSPHATE SODIUM'
_chemical_properties_physical    Heat-sensitive
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_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_method           SHELXL-97
_audit_update_record
;
2014-09-29 deposited with the CCDC.
2016-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.5585(12)
_cell_length_b                   7.0470(13)
_cell_length_c                   38.869(7)
_cell_measurement_reflns_used    7116
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.94
_cell_volume                     1796.4(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            12569
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_T_max  0.9476
_exptl_absorpt_correction_T_min  0.9385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone and water'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.08(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3174
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0499
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+1.6134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1397
_reflns_number_gt                3059
_reflns_number_total             3174
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ce00034g2.cif
_cod_data_source_block           mo_20140917campna2_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7223962--7223963.cif.
;
_cod_original_sg_symbol_H-M      'P2(1)2(1)2(1) '
_cod_database_code               7223962