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_7055490
_publ_section_title
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 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 H36 Cl Cu2 N8 O5, C20 H36 Cu2 N8 O, 2(Cl O4), Cl0.5 O2.41, 2(H2 O), Cl0.5 O1.59'
_chemical_formula_sum            'C40 H76 Cl4 Cu4 N16 O20'
_chemical_formula_weight         1497.12
_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             2016-03-14
_audit_creation_method
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Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
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_audit_update_record
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2016-03-15 deposited with the CCDC.
2016-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                88.419(3)
_cell_angle_beta                 80.246(4)
_cell_angle_gamma                70.061(4)
_cell_formula_units_Z            2
_cell_length_a                   12.0759(5)
_cell_length_b                   14.4835(6)
_cell_length_c                   18.6853(8)
_cell_measurement_reflns_used    7335
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      27.3760
_cell_measurement_theta_min      3.2170
_cell_volume                     3026.2(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector_area_resol_mean 16.0267
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Sapphire3'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17350
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.925
_exptl_absorpt_coefficient_mu    1.646
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       block
_exptl_crystal_F_000             1544
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     902
_refine_ls_number_reflns         10400
_refine_ls_number_restraints     83
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0535P)^2^+5.1202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1309
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8399
_reflns_number_total             10400
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03234b2.cif
_cod_data_source_block           Compound_3
_cod_depositor_comments
'Adding full bibliography for 7055486--7055490.cif.'
_cod_database_code               7055490
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H5A,H5B} of O5, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  {H2C,H2D} of O2, {H1C,H1D} of O1, {H4C,H4D} of O4, {H3C,H3D} of O3
2. Restrained distances
 H2C-O2 = H2D-O2
 0.82 with sigma of 0.01
 O5-H5A = O5-H5B
 0.85 with sigma of 0.01
 H4D-H16_$1
 2.2 with sigma of 0.01
 H4D-O4
 0.85 with sigma of 0.01
 H4C-O4
 0.85 with sigma of 0.01
 H13B-H1C
 2.2 with sigma of 0.01
 Cl4-O46 \\sim Cl4-O44 \\sim Cl4-O42 \\sim Cl4-O48
 with sigma of 0.02
 O46-O44 \\sim O46-O42 \\sim O46-O48
 with sigma of 0.1
3. Rigid bond restraints
 Cl4, O41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl4, O48
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl4, O42
 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
 Cu2, O48
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cu4, O11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O46, Cl4
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 O42, Cl4
 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(O28) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O48) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O53) \\sim Ueq, Uanis(Cl1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(O44) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O14) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O46) \\sim Ueq, Uanis(O42) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
5. Others
 Sof(O42)=Sof(O44)=Sof(O46)=Sof(O48)=1-FVAR(1)
 Sof(O45)=Sof(O47)=Sof(O43)=Sof(O41)=FVAR(1)
 Sof(O13)=Sof(O11)=Sof(O12)=Sof(O14)=1-FVAR(2)
 Sof(O52)=Sof(O54)=Sof(O53)=Sof(O51)=FVAR(2)
 Sof(O28)=Sof(O22)=Sof(O24)=Sof(O26)=1-FVAR(3)
 Sof(O27)=Sof(O25)=Sof(O23)=Sof(O21)=FVAR(3)
 Fixed Sof: Cl5(0.5) O2(0.5) H2C(0.5) H2D(0.5) O1(0.5) H1C(0.5) H1D(0.5)
 Cl1(0.5)
6.a Free rotating group:
 O3(H3C,H3D), O1(H1C,H1D)
6.b Rotating group with stretchable bonds:
 O5(H5A,H5B), O4(H4C,H4D)
6.c Ternary CH refined with riding coordinates:
 N8(H8), N1(H1), N5(H5), N4(H4), N12(H12), N9(H9), N13(H13), N16(H16)
6.d Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C1(H1A,H1B), C31(H31A,H31B), C24(H24A,H24B), C11(H11A,H11B),
 C22(H22A,H22B), C33(H33A,H33B), C13(H13A,H13B), C3(H3A,H3B), C5(H5C,H5D),
 C35(H35A,H35B), C32(H32A,H32B), C21(H21A,H21B), C34(H34A,H34B), C12(H12A,H12B),
  C9(H9A,H9B), C36(H36A,H36B), C23(H23A,H23B), C15(H15A,H15B), C25(H25A,H25B),
 C26(H26A,H26B), C2(H2A,H2B), C14(H14A,H14B), C19(H19A,H19B), C30(H30A,H30B),
 C40(H40A,H40B), C20(H20A,H20B), C10(H10A,H10B)
6.e Aromatic/amide H refined with riding coordinates:
 C17(H17), C28(H28), C38(H38), C7(H7)
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_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method water