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_7030973
_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         'C74 H60 N6 O12 P2 V3'
_chemical_formula_sum            'C74 H60 N6 O12 P2 V3'
_chemical_formula_weight         1440.04
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-04-07
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.213(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.464(5)
_cell_length_b                   27.628(5)
_cell_length_c                   14.057(5)
_cell_measurement_reflns_used    3505
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.14
_cell_measurement_theta_min      2.34
_cell_volume                     10275(5)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0793
_diffrn_reflns_av_unetI/netI     0.0936
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            27622
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.067
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.378173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0634 before and 0.0316 after correction.
The Ratio of minimum to maximum transmission is 0.3782.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    0.931
_exptl_crystal_description       block
_exptl_crystal_F_000             2964
_exptl_crystal_size_max          0.088
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.078
_refine_diff_density_max         1.237
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         9723
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1673
_refine_ls_R_factor_gt           0.1179
_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          0.3111
_refine_ls_wR_factor_ref         0.3460
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4928
_reflns_number_total             9723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt00720d2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7030970--7030975.cif.'
_cod_database_code               7030973
_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 O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C20) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C1Z) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.002
Uanis(C1U) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
Uanis(C1S) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H9A(0.5) H9B(0.5) H11A(0.5) H11B(0.5)
4.a Riding coordinates:
 O9(H9A,H9B), O11(H11A,H11B)
4.b Rotating group:
 O5(H5A,H5B)
4.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C16(H16), C17(H17), C1A(H1A), C1F(H1F), C1G(H1G),
 C1H(H1H), C1I(H1I), C1J(H1J), C1K(H1K), C1L(H1L), C1M(H1M), C1N(H1N), C1O(H1O),
  C1P(H1P), C1R(H1R), C1S(H1S), C1T(H1T), C1U(H1U), C1V(H1V), C1W(H1W),
 C1X(H1X), C1Z(H1Z), C1Y(H1Y), C20(H20), C2(H2)
;