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_7055488
_publ_section_title
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 A water molecule in the interior of a 1H-pyrazole Cu2+metallocage
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_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         '2(C20 H34 Cu2 N8), 4(Cl O4), H2 O'
_chemical_formula_sum            'C40 H70 Cl4 Cu4 N16 O17'
_chemical_formula_weight         1443.08
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-01-06
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-11-14 deposited with the CCDC.
2016-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.7230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.5030(7)
_cell_length_b                   14.4620(4)
_cell_length_c                   17.1670(4)
_cell_measurement_reflns_used    5800
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      0.998
_cell_volume                     5713.4(3)
_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, 2008)'
_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  0.0406
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9815
_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         24.998
_diffrn_reflns_theta_min         1.770
_exptl_absorpt_coefficient_mu    1.736
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       block
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.739
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5033
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0717
_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^)+(0.1381P)^2^+9.3643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1991
_refine_ls_wR_factor_ref         0.2247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3225
_reflns_number_total             5033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03234b2.cif
_cod_data_source_block           COMPOUND2
_cod_depositor_comments
'Adding full bibliography for 7055486--7055490.cif.'
_cod_database_code               7055488
_shelxl_version_number           SHELXL-97
_olex2_refinement_description
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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,H) groups
2. Restrained distances
 H1Bb-H7Bb
 2.1 with sigma of 0.01
3. Rigid bond restraints
 C9, C8
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 C5B, C4B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2B, N4B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl3, O33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N3B, C6B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N4B, C2B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C10, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O24B \\sim O23B \\sim O22B \\sim O21B \\sim Cl22: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
N2B \\sim C5B \\sim C4B: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
N1 \\sim C2 \\sim C3: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C7B \\sim N3B \\sim C8B: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.01
N3B \\sim C5B \\sim C6B: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.01
C7 \\sim C8 \\sim C9: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Cl1 \\sim O12 \\sim O11: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C1 \\sim C10 \\sim N1: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.01
C7B \\sim N3B \\sim C6B \\sim C5B: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(O22) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.1
5. Others
 Fixed Sof: O33(0.5) O34(0.5) O32(0.5) O1(0.5) H1c(0.5) H1d(0.5) O24(0.5)
 O23(0.5) O22(0.5) O21(0.5) Cl2(0.5) O24B(0.5) O23B(0.5) O22B(0.5) O21B(0.5)
 Cl22(0.5)
 Fixed X: Cl1(0)
 Fixed Z: Cl1(0.75)
6.a Free rotating group:
 O1(H1c,H1d)
6.b Ternary CH refined with riding coordinates:
 N4(H4), N1(H1), N4B(H4B), N3B(H3B)
6.c Secondary CH2 refined with riding coordinates:
 C7(H7a,H7b), C6(H6a,H6b), C7B(H7Ba,H7Bb), C2(H2a,H2b), C10(H10a,H10b),
 C8B(H8Ba,H8Bb), C9B(H9Ba,H9Bb), C10B(H10c,H10d), C6B(H6Ba,H6Bb), C1(H1a,H1b),
 C8(H8a,H8b), C2B(H2Ba,H2Bb), C9(H9a,H9b), C1B(H1Ba,H1Bb)
6.d Aromatic/amide H refined with riding coordinates:
 C4(H4a), C4B(H4Ba)
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