Di-, tri- and tetranuclear molecular vanadium phosphonates: a chloride encapsulated tetranuclear bowl.
Sahoo, Dipankar; Suriyanarayanan, Ramakirushnan; Chandrasekhar, Vadapalli; Dalton transactions (Cambridge, England : 2003) 43 (2014) 10898–10909; doi:10.1039/c4dt00720d

data_7030972
_publ_section_title
;
 Di-, tri- and tetranuclear molecular vanadium phosphonates: a chloride
 encapsulated tetranuclear bowl.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10898
_journal_page_last               10909
_journal_paper_doi               10.1039/c4dt00720d
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         '2(C24 H25 N4 O7 P V2), 3(C H4 O)'
_chemical_formula_sum            'C51 H62 N8 O17 P2 V4'
_chemical_formula_weight         1324.78
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2014-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                66.947(5)
_cell_angle_beta                 84.914(6)
_cell_angle_gamma                80.991(5)
_cell_formula_units_Z            1
_cell_length_a                   9.765(3)
_cell_length_b                   12.448(4)
_cell_length_c                   14.734(4)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.58
_cell_volume                     1626.9(8)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_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 (Burla et al., 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0937
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10470
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         4.205
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.673
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.400757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0848 before and 0.0338 after correction.
The Ratio of minimum to maximum transmission is 0.4008.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       block
_exptl_crystal_F_000             682
_exptl_crystal_size_max          0.068
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.477
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5608
_refine_ls_number_restraints     121
_refine_ls_restrained_S_all      1.284
_refine_ls_R_factor_all          0.1292
_refine_ls_R_factor_gt           0.0967
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2693
_refine_ls_wR_factor_ref         0.3054
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3588
_reflns_number_total             5608
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt00720d2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7030970--7030975.cif.'
_cod_database_code               7030972
_shelxl_version_number           2013-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O9-C27
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(V2) \\sim Ueq, Uanis(V1) \\sim Ueq, Uanis(P1) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.002
Uanis(O9) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(O4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C24)
\\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5) O9(0.5) H9A(0.5)
5.a Riding coordinates:
 O9(H9A)
5.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C1(H1), C2(H2), C14(H14), C10(H10), C17(H17), C4(H4), C3(H3), C8(H8),
 C13(H13), C19(H19), C7(H7), C11(H11), C12(H12), C18(H18), C20(H20)
5.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C)
5.d Idealised tetrahedral OH refined as rotating group:
 O8(H8A)
;