A single but hydrogen-bonded water molecule confined in an anisotropic subnanospace.
Hashikawa, Yoshifumi; Hasegawa, Shota; Murata, Yasujiro; Chemical communications (Cambridge, England) 54 (2018) 13686–13689; doi:10.1039/c8cc07339b

data_7122603
_publ_section_title
;
 A single but hydrogen-bonded water molecule confined in an anisotropic
 subnanospace.
;
_journal_issue                   97
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13686
_journal_page_last               13689
_journal_paper_doi               10.1039/c8cc07339b
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C130 H89.64 N6 Ni O4.67 S'
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_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
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_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-07-24 deposited with the CCDC.
2018-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                91.943(2)
_cell_angle_beta                 109.228(2)
_cell_angle_gamma                108.323(2)
_cell_formula_units_Z            2
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_cell_length_b                   17.675(2)
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_cell_measurement_reflns_used    15751
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.01
_cell_measurement_theta_min      1.04
_cell_volume                     4566.9(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker Smart APEX II'
_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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
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_diffrn_reflns_limit_l_min       -24
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_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    0.303
_exptl_absorpt_correction_T_max  0.9791
_exptl_absorpt_correction_T_min  0.9066
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1986
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.201
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1374
_refine_ls_number_reflns         15751
_refine_ls_number_restraints     3
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_refine_ls_R_factor_all          0.0896
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_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0770P)^2^+7.2746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1745
_reflns_number_gt                11719
_reflns_number_total             15751
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8cc07339b2.cif
_cod_data_source_block           1S17H3_NiP_a
_cod_depositor_comments
'Adding full bibliography for 7122602--7122603.cif.'
_cod_original_cell_volume        4566.8(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7122603