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_7055486
_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 H34 Cu2 N8, C40 H72 Cu4 N16 O2, 6(Cl O4), 3(H2 O)'
_chemical_formula_sum            'C60 H112 Cl6 Cu6 N24 O29'
_chemical_formula_weight         2227.67
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-15
_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            4
_cell_length_a                   28.487(2)
_cell_length_b                   24.612(4)
_cell_length_c                   12.984(5)
_cell_measurement_reflns_used    271756
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      0.407
_cell_volume                     9103(4)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.835
_diffrn_measured_fraction_theta_max 0.835
_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  0.1028
_diffrn_reflns_av_unetI/netI     0.1513
_diffrn_reflns_Laue_measured_fraction_full 0.835
_diffrn_reflns_Laue_measured_fraction_max 0.835
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            19856
_diffrn_reflns_point_group_measured_fraction_full 0.835
_diffrn_reflns_point_group_measured_fraction_max 0.835
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.003
_diffrn_reflns_theta_min         1.652
_exptl_absorpt_coefficient_mu    1.640
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_description       block
_exptl_crystal_F_000             4592
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.889
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         6874
_refine_ls_number_restraints     393
_refine_ls_restrained_S_all      0.895
_refine_ls_R_factor_all          0.2355
_refine_ls_R_factor_gt           0.0811
_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^)+(0.1557P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2095
_refine_ls_wR_factor_ref         0.2836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2256
_reflns_number_total             6874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj03234b2.cif
_cod_data_source_block           Compound_2B
_cod_depositor_comments
'Adding full bibliography for 7055486--7055490.cif.'
_cod_database_code               7055486
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H1C,H1D} of O1, {H4A,H4B} of O4, All C(H,H) groups, All
  N(H) groups
 At 1.5 times of:
  {H3A,H3B} of O3, {H2A,H2B} of O2
2. Restrained distances
 O4-H4A
 0.82 with sigma of 0.02
 O4-H4B
 0.82 with sigma of 0.02
 N7-H1C
 2.92 with sigma of 0.01
 H1C-O1
 0.82 with sigma of 0.01
 O1-H1D
 0.82 with sigma of 0.01
 C30-C31
 1.45 with sigma of 0.01
 C47-C48
 1.45 with sigma of 0.01
 H1D-O33
 2.22 with sigma of 0.02
 O3-H3B
 0.82 with sigma of 0.01
 O3-H3B
 0.82 with sigma of 0.01
 H3B_$1-H2B
 2.2 with sigma of 0.01
 H4B-H4A
 1.5 with sigma of 0.04
 O13-O15 \\sim O13-O16 \\sim O15-O16
 with sigma of 0.02
 Cl1-O15 \\sim Cl1-O16 \\sim Cl1-O17 \\sim Cl1-O18
 with sigma of 0.02
 O12-O13 \\sim O12-O15 \\sim O12-O16
 with sigma of 0.02
 Cl1-O11 \\sim Cl1-O12 \\sim Cl1-O13 \\sim Cl1-O14
 with sigma of 0.02
 O24-O21 \\sim O24-O26 \\sim O24-O27 \\sim O21-O26 \\sim O21-O27 \\sim O26-O27
 with sigma of 0.02
 O21-O22 \\sim O21-O23 \\sim O21-O25 \\sim O22-O23 \\sim O22-O25 \\sim O23-O25
 with sigma of 0.02
3. Rigid bond restraints
 C46, C47
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C43, C42, C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, C3, C4, C5, C6, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N8, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C25, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N8, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C44, C45, N12, Cu4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C30, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C51, C50
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C44, C42, N11, N10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N4, C6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2, O24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C41, N9, C51
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C44, C43
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl1, O11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl3, O32
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2, O25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cu2, N4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O22, Cl2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cu2, N6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2, Cu2, Cl1, O14
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 O18, Cl1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O27, Cl2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N6, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C10, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl1, O12, O16, O14, O17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N11 \\sim N10: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C46 \\sim C47 \\sim C48: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C43 \\sim C42 \\sim C41: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C2 \\sim C3 \\sim C6 \\sim C7: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C44 \\sim C45 \\sim N12 \\sim Cu4: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C51 \\sim C50 \\sim C49 \\sim N9: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.05
N12 \\sim C46 \\sim C47: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.06
C22 \\sim C23 \\sim C21 \\sim N8 \\sim C31: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.05
C10 \\sim C11 \\sim C9: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
Cl1 \\sim O15 \\sim O13: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C28 \\sim C27: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C5 \\sim C4 \\sim N4: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
Cl4 \\sim O45: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
Cl4 \\sim O45 \\sim O43 \\sim O41: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.04
O26 \\sim O22 \\sim O21 \\sim O25 \\sim O24: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
Cl1 \\sim O16 \\sim O17 \\sim O13: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(O42) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.2
Uanis(O43) \\sim Ueq, Uanis(O44) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.04
Uanis(O31) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O1)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.05
Uanis(O44) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O18) \\sim Ueq, Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(O12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(O17) \\sim Ueq, Uanis(O41) \\sim Ueq, Uanis(O45) \\sim Ueq, Uanis(O27)
\\sim Ueq, Uanis(O33) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.1
5. Others
 Fixed Sof: O16(0.75) O12(0.75) O15(0.75) O4(0.5) H4A(0.5) H4B(0.5) O27(0.5)
 O26(0.5) O43(0.25) O41(0.5) O13(0.75) O23(0.5) O42(0.5) O24(0.5) O22(0.5)
 H1C(0.5) O14(0.25) O11(0.25) O17(0.25) O3(0.5) H3A(0.5) H3B(0.5) O25(0.5)
 O44(0.25) O18(0.25)
6.a Rotating group:
 O2(H2A,H2B)
6.b Rotating group with stretchable bonds:
 O4(H4A,H4B), O1(H1C,H1D), O3(H3A,H3B)
6.c Ternary CH refined with riding coordinates:
 N9(H9), N5(H5), N1(H1), N12(H12), N4(H4), N8(H8)
6.d Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C28(H28A,H28B), C25(H25A,H25B), C9(H9A,H9B), C10(H10A,H10B),
 C11(H11A,H11B), C41(H41A,H41B), C7(H7A,H7B), C51(H51A,H51B), C6(H6A,H6B),
 C45(H45A,H45B), C1(H1A,H1B), C46(H46A,H46B), C26(H26A,H26B), C27(H27A,H27B),
 C8(H8A,H8B), C50(H50A,H50B), C30(H30A,H30B), C29(H29A,H29B), C31(H31A,H31B),
 C21(H21A,H21B), C49(H49A,H49B), C47(H47A,H47B), C48(H48A,H48B)
6.e Aromatic/amide H refined with riding coordinates:
 C43(H43), C23(H23), C3(H3)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'