A water molecule in the interior of a 1H-pyrazole Cu2+metallocage
Pitarch-Jarque, Javier; Belda, Raquel; Blasco, Salvador; Navarro, Pilar; Tejero, Roberto; Junquera-Hernández, José Miguel; Pérez-Mondéjar, Vicente; García-España, Enrique; New J. Chem. 40 (2016) 5670–; doi:10.1039/C5NJ03234B

data_7055487
_publ_section_title
;
 A water molecule in the interior of a 1H-pyrazole Cu2+metallocage
;
_journal_issue                   7
_journal_name_full               'New J. Chem.'
_journal_page_first              5670
_journal_paper_doi               10.1039/C5NJ03234B
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C20 H38 N8, 2(Cl O4)'
_chemical_formula_sum            'C20 H38 Cl2 N8 O8'
_chemical_formula_weight         589.48
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-11-14 deposited with the CCDC.
2016-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                65.970(2)
_cell_angle_beta                 89.173(2)
_cell_angle_gamma                70.563(2)
_cell_formula_units_Z            1
_cell_length_a                   8.9190(3)
_cell_length_b                   9.3360(4)
_cell_length_c                   9.7410(3)
_cell_measurement_reflns_used    3134
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     691.66(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_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    Sir97
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4750
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.446
_exptl_absorpt_coefficient_mu    0.293
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       block
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2441
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0696P)^2^+0.3517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1403
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1937
_reflns_number_total             2441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03234b2.cif
_cod_data_source_block           COMPOUND1
_cod_depositor_comments
'Adding full bibliography for 7055486--7055490.cif.'
_cod_database_code               7055487
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
2. Restrained distances
 N4-H4
 0.9 with sigma of 0.02
 N3-H3
 0.9 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1B) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: O4B(0.5) O1B(0.5) O2B(0.5) O3B(0.5) Cl1B(0.5) O4A(0.5) O1A(0.5)
 O2A(0.5) O3A(0.5) Cl1(0.5)
5.a Riding coordinates:
 C1(H1c,H1d), C7(H7a,H7b), C10(H10a,H10b), C2(H2a,H2b), C6(H6a,H6b), C4(H4a),
 C9(H9a,H9b), C8(H8a,H8b)
5.b Rotating group with stretchable bonds:
 N3(H3), N4(H4)
5.c Secondary CH2 refined with riding coordinates:
 N1(H1a,H1b)
;
_olex2_submission_special_instructions 'No special instructions were received'