Using a flexible bis(pyrazol) ligand to construct four new Keggin-based compounds: syntheses, structures and properties
Tian, Aixiang; Ni, Huaiping; Ji, Xuebin; Tian, Yan; Liu, Guocheng; Ying, Jun; RSC Adv. 7 (2017) 5774–; doi:10.1039/C6RA25156K

data_7227482
_publ_section_title
;
 Using a flexible bis(pyrazol) ligand to construct four new Keggin-based
 compounds: syntheses, structures and properties
;
_journal_issue                   10
_journal_name_full               'RSC Adv.'
_journal_page_first              5774
_journal_paper_doi               10.1039/C6RA25156K
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C44 H60 Cu2 N16 O80 P2 W24, 2(H2 O)'
_chemical_formula_sum            'C44 H72 Cu2 N16 O82 P2 W24'
_chemical_formula_weight         6738
_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             2016-09-03
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2016-10-10 deposited with the CCDC.
2017-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                94.102(4)
_cell_angle_beta                 105.644(4)
_cell_angle_gamma                101.451(3)
_cell_formula_units_Z            1
_cell_length_a                   12.444(2)
_cell_length_b                   14.557(3)
_cell_length_c                   17.393(3)
_cell_measurement_reflns_used    4498
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.657
_cell_measurement_theta_min      2.454
_cell_volume                     2947.4(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      293.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.1140
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16257
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.227
_exptl_absorpt_coefficient_mu    23.787
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.792
_exptl_crystal_description       block
_exptl_crystal_F_000             2960
_refine_diff_density_max         4.178
_refine_diff_density_min         -4.865
_refine_diff_density_rms         0.542
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         10398
_refine_ls_number_restraints     1023
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0705
_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^)+(0.1210P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1829
_refine_ls_wR_factor_ref         0.2172
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6356
_reflns_number_total             10398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ra25156k2.cif
_cod_data_source_block           compound-2
_cod_original_cell_volume        2947.5(10)
_cod_database_code               7227482
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(P1) \\sim Ueq, Uanis(P2) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.001
Uanis(O25) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.001
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: P1(0.5) O1(0.5) O2(0.5) O3(0.5) O4(0.5) O23(0.5) O24(0.5) O25(0.5)
 O26(0.5)
5.a Riding coordinates:
 O1W(H1WA,H1WB)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C17(H17A,H17B)
5.c Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C)
5.d Aromatic/amide H refined with riding coordinates:
 N2(H2), N6(H6)
;
_shelx_fab_checksum              28033
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'