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_7055489
_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
'2(C20 H34 Cu2 N8), 2(C40 H71 Cu4 N16 O2), 12(Cl O4), 9(H2 O)'
_chemical_formula_sum            'C120 H228 Cl12 Cu12 N48 O61'
_chemical_formula_weight         4507.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-03-15 deposited with the CCDC.
2016-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   28.221(3)
_cell_length_b                   24.265(10)
_cell_length_c                   12.8478(9)
_cell_measurement_reflns_used    1702
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      22.4770
_cell_measurement_theta_min      3.1760
_cell_volume                     8798(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0267
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset, Sapphire3'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1184
_diffrn_reflns_av_unetI/netI     0.1579
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            24182
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.887
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.699
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32091
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_description       block
_exptl_crystal_F_000             4648
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         7911
_refine_ls_number_restraints     225
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.2546
_refine_ls_R_factor_gt           0.0996
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1428P)^2^+4.3115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2376
_refine_ls_wR_factor_ref         0.3457
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2642
_reflns_number_total             7911
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03234b2.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
'Adding full bibliography for 7055486--7055490.cif.'
_cod_database_code               7055489
_oxdiff_exptl_absorpt_empirical_full_min 0.618
_oxdiff_exptl_absorpt_empirical_full_max 2.439
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_olex2_refinement_description
;
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
 C11-C10
 1.48 with sigma of 0.01
 C10-C9
 1.45 with sigma of 0.01
 C9-N4
 1.43 with sigma of 0.01
 H1D-O1
 0.85 with sigma of 0.01
 H1C-O1
 0.85 with sigma of 0.01
 H4C-O11_$1
 2.37 with sigma of 0.01
 C31_$1-N12_$1
 1.55 with sigma of 0.01
 H4D-H31A
 2.19 with sigma of 0.01
 H31A-H4C
 2.19 with sigma of 0.01
 H4C-H25A_$1
 2.18 with sigma of 0.01
 H3C-O23
 2.55 with sigma of 0.01
 H3C-H12
 2.19 with sigma of 0.01
 C32-C33
 1.45 with sigma of 0.01
 H19A-H4BB
 2.2 with sigma of 0.01
 O31-O34 \\sim O31-O33 \\sim O31-O36 \\sim O34-O33 \\sim O34-O36 \\sim O33-O36
 with sigma of 0.02
 Cl3-O34 \\sim Cl3-O31 \\sim Cl3-O33 \\sim Cl3-O36
 with sigma of 0.02
 Cl3-O35 \\sim Cl3-O32 \\sim Cl3-O37
 with sigma of 0.02
3. Rigid bond restraints
 C10, C11, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2, O22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C24, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C21, C22, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cu1, N1
 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
 N8, C20
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cu3, N10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N4, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C31, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C33, C32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cu1, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N9, C26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N5, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N8, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2, O23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(N4) \\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim
Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(N6) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C3)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(O12) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.1
Uanis(C1) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O22)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.05
Uanis(O4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.1
Uanis(C11) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C23)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(O42) \\sim Ueq, Uanis(C33) \\sim Ueq,
Uanis(C5) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O34) \\sim Ueq, Uanis(O35) \\sim Ueq, Uanis(O32) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.04
Uanis(O33) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.1
Uanis(O37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: H9B(0.5) O3(0.75) H3C(0.75) H3D(0.75) O4B(0.66666) H4BA(0.66666)
 H4BB(0.66666) H1C(0.5) H1D(0.5) O4(0.33333) H4C(0.33333) H4D(0.33333) O37(0.5)
 O35(0.5) O33(0.5) O36(0.5) O32(0.5) O34(0.5)
6.a Free rotating group:
 O3(H3C,H3D), O4B(H4BA,H4BB), O4(H4C,H4D)
6.b Rotating group:
 O2(H2A,H2B)
6.c Rotating group with stretchable bonds:
 O1(H1C,H1D)
6.d Ternary CH refined with riding coordinates:
 N9(H9), N5(H5), N8(H8), N4(H4), N1(H1), N12(H12)
6.e Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C21(H21A,H21B), C14(H14A,H14B), C13(H13A,H13B), C1(H1A,H1B),
 C12(H12A,H12B), C22(H22A,H22B), C2(H2C,H2D), C24(H24A,H24B), C15(H15A,H15B),
 C10(H10A,H10B), C23(H23A,H23B), C19(H19A,H19B), C4(H4A,H4B), C20(H20A,H20B),
 C3(H3A,H3B), C30(H30A,H30B), C25(H25A,H25B), C11(H11A,H11B), C9(H9A,H9B),
 C8(H8A,H8B), C33(H33A,H33B), C31(H31A,H31B), C32(H32A,H32B)
6.f Aromatic/amide H refined with riding coordinates:
 C28(H28), C17(H17), C6(H6)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method water