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_7030970
_publ_section_title
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 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         'C32 H40 N4 O10 P2 V2, 2(Cl)'
_chemical_formula_sum            'C32 H40 Cl2 N4 O10 P2 V2'
_chemical_formula_weight         875.40
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-05
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.079(5)
_cell_length_b                   18.583(5)
_cell_length_c                   10.924(5)
_cell_measurement_reflns_used    2632
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.94
_cell_measurement_theta_min      2.19
_cell_volume                     3873(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1282
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19242
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.19
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.078127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.1488 before and 0.0496 after correction. The Ratio of minimum to maximum transmission is 0.0781. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.084
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.080
_refine_diff_density_min         -1.516
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0727P)^2^+7.0044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.1670
_reflns_number_gt                2816
_reflns_number_total             3652
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00720d2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7030970--7030975.cif.'
_cod_database_code               7030970
_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. Uiso/Uaniso restraints and constraints
Uanis(O6) = Uanis(O2)
Uanis(C9) = Uanis(C8)
3. Others
 Fixed Sof: H14B(0.5) H14C(0.5) H17A(0.5) H17B(0.5) H17C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6A), C7(H7), C10(H10), C11(H11), C12(H12)
4.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C)
4.c Idealised tetrahedral OH refined as rotating group:
 O2(H2A), O6(H6)
;