Neutral and anionic phosphate-diesters as molecular templates for the encapsulation of a water dimer.
Gupta, Vivek; Santra, Biswajit; Mandal, Debdeep; Das, Shubhajit; Narayanan, Ramakirushnan Suriya; Kalita, Pankaj; Rao, D. Krishna; Schulzke, Carola; Pati, Swapan K.; Chandrasekhar, Vadapalli; Jana, Anukul; Chemical communications (Cambridge, England) 54 (2018) 11913–11916; doi:10.1039/c8cc07138a

data_7122383
_publ_section_title
;
 Neutral and anionic phosphate-diesters as molecular templates for the
 encapsulation of a water dimer.
;
_journal_issue                   84
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11913
_journal_page_last               11916
_journal_paper_doi               10.1039/c8cc07138a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C70 H63 O4 P, 2(H2 O)'
_chemical_formula_sum            'C70 H67 O6 P'
_chemical_formula_weight         1035.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-24
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-30 deposited with the CCDC.
2018-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.195(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6501(3)
_cell_length_b                   37.3357(7)
_cell_length_c                   14.6867(3)
_cell_measurement_reflns_used    26641
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.6710
_cell_measurement_theta_min      2.7410
_cell_volume                     5793.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            61616
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.500
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         2.519
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       block
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.323
_exptl_crystal_size_min          0.204
_refine_diff_density_max         1.340
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         11997
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+2.7644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1177
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9728
_reflns_number_total             11997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07138a2.cif
_cod_data_source_block           AJ0030
_cod_depositor_comments
'Adding full bibliography for 7122383--7122386.cif.'
_cod_database_code               7122383
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O5-H5A = O5-H5B = O6-H6A = O6-H6B
 0.96 with sigma of 0.02
 H5A-H5B = H6A-H6B
 1.52 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C42(H42), C43(H43), C44(H44)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C25(H25), C26(H26), C27(H27), C28(H28),
  C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C38(H38),
 C40(H40), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53),
  C54(H54), C55(H55), C56(H56), C60(H60), C61(H61), C62(H62), C63(H63),
 C64(H64), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70)
3.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C57(H57A,H57B,H57C), C58(H58A,H58B,
 H58C)
3.d Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              19361
_shelx_hkl_checksum              91410
_olex2_submission_special_instructions 'No special instructions were received'