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_7030971
_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         'C28 H41 N4 O11 P2 V2, 2(Cl)'
_chemical_formula_sum            'C28 H41 Cl2 N4 O11 P2 V2'
_chemical_formula_weight         844.37
_chemical_name_systematic
;
 ?
;
_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             2014-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.066(5)
_cell_length_b                   14.961(5)
_cell_length_c                   10.893(5)
_cell_measurement_reflns_used    3565
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.23
_cell_volume                     3759(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0585
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19194
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.345
_diffrn_reflns_theta_min         4.078
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.503776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0440 before and 0.0268 after correction.
The Ratio of minimum to maximum transmission is 0.5038.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       block
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.082
_refine_diff_density_max         2.288
_refine_diff_density_min         -1.255
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3570
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.1351
_refine_ls_R_factor_gt           0.1182
_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^)+(0.1054P)^2^+64.1964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2723
_refine_ls_wR_factor_ref         0.2865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2939
_reflns_number_total             3570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt00720d2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7030970--7030975.cif.'
_cod_database_code               7030971
_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 C(H,H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C16-C14
 1.54 with sigma of 0.02
 C15-C14
 1.54 with sigma of 0.02
 C14-C17
 1.54 with sigma of 0.02
 H6A-O6
 0.83 with sigma of 0.02
 C17-C16
 2.5 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C13) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.002
Uanis(C3) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
Uanis(O6) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
Uanis(C16) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(C17) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.002
Uanis(O2) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.002
Uanis(Cl1) \\sim Ueq, Uanis(Cl2) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.002
Uanis(O5) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.002
Uanis(O4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: H15A(0.5) H15B(0.5) H15C(0.5) H3C(0.5) H3D(0.5) H3E(0.5) C16(0.5)
 H16A(0.5) H16B(0.5) H16C(0.5) C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5)
5.a Riding coordinates:
 C3(H3C,H3D,H3E)
5.b Rotating group:
 O3(H3A,H3B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C10(H10), C6(H6), C5(H5), C13(H13), C11(H11), C12(H12)
5.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
5.e Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;