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_7030975
_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
'C80 H72 O20 P4 V4, Cl, C5 H9 N2, 3(C7 H8)'
_chemical_formula_sum            'C106 H105 Cl N2 O20 P4 V4'
_chemical_formula_weight         2090.00
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                 98.390(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.502(5)
_cell_length_b                   32.938(5)
_cell_length_c                   39.238(5)
_cell_measurement_reflns_used    4667
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.22
_cell_measurement_theta_min      2.23
_cell_volume                     21099(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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.1248
_diffrn_reflns_av_unetI/netI     0.1609
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            121159
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.850
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.567226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0571 before and 0.0444 after correction.
The Ratio of minimum to maximum transmission is 0.5672.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       block
_exptl_crystal_F_000             8672
_exptl_crystal_size_max          0.088
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.991
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2449
_refine_ls_number_reflns         39165
_refine_ls_number_restraints     258
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.1959
_refine_ls_R_factor_gt           0.0949
_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^)+(0.1316P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2282
_refine_ls_wR_factor_ref         0.2796
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16890
_reflns_number_total             39165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_original_formula_sum            'C212 H210 Cl2 N4 O40 P8 V8'
_cod_original_formula_weight         4180.01
_cod_original_formula_units_Z            4
_cod_original_formula_moiety
'2(C80 H72 O20 P4 V4, Cl, C5 H9 N2), 6(C7 H8)'
_cod_depositor_comments
;
Adding full bibliography for 7030970--7030975.cif.

2017-03-01
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_data_source_file            c4dt00720d2.cif
_cod_data_source_block           6
_cod_database_code               7030975
_shelxl_version_number           2013-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C50) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C5B)
\\sim Ueq, Uanis(C5H) \\sim Ueq, Uanis(C5I) \\sim Ueq, Uanis(C5G) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C58) \\sim Ueq, Uanis(C4R) \\sim Ueq, Uanis(C3G) \\sim Ueq, Uanis(C2X)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C4K) \\sim Ueq, Uanis(C3U) \\sim Ueq, Uanis(C4X) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C54) \\sim Ueq, Uanis(C4V) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C4U)
\\sim Ueq, Uanis(C4M) \\sim Ueq, Uanis(C4P) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C3D) \\sim Ueq, Uanis(C4Z) \\sim Ueq, Uanis(C4I) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C4N) \\sim Ueq, Uanis(C4G) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C47) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C1F) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2M) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(C48) \\sim Ueq, Uanis(C5E) \\sim Ueq, Uanis(C5O) \\sim Ueq, Uanis(C5K)
\\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C4W) \\sim Ueq: with sigma of 0.004 and
sigma for terminal atoms of 0.002
Uanis(C3Q) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C3V) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C4C) \\sim Ueq, Uanis(C4F) \\sim Ueq, Uanis(C4E) \\sim Ueq: with sigma of
0.006 and sigma for terminal atoms of 0.002
Uanis(C23) \\sim Ueq, Uanis(C3Q) \\sim Ueq, Uanis(C4T) \\sim Ueq, Uanis(C3L)
\\sim Ueq: with sigma of 0.006 and sigma for terminal atoms of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 N58(H58), C70(H70), C73(H73), C75(H75), C78(H78), C80(H80), C84(H84),
 C86(H86), C87(H87), N88(H88), C89(H89), C90(H90), C91(H91), C92(H92), C94(H94),
  C95(H95), C96(H96), C97(H97), C98(H98), C99(H99), N10(H10), C1(H1), C4(H4),
 C7(H7), C8(H8), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C1A(H1A), C1B(H1B), C1C(H1C), C1D(H1D), C1E(H1E), C1I(H1I), C1K(H1K),
  C1L(H1L), C1M(H1M), C1O(H1O), C1P(H1P), C1S(H1S), C1V(H1V), C1W(H1W),
 C1X(H1X), C1Y(H1Y), C1Z(H1Z), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C27(H27), N29(H29), C2C(H2C), C2D(H2D), C2E(H2E),
 C2F(H2F), C2G(H2G), C2H(H2H), C2I(H2I), C2L(H2L), C2N(H2N), C2O(H2O), C2P(H2P),
  C2Q(H2Q), C2R(H2R), C2S(H2S), C2T(H2T), C2U(H2U), C2W(H2W), C2Y(H2Y),
 C2Z(H2Z), C30(H30), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
  C39(H39), C3A(H3AA), C3B(H3B), C3C(H3CA), C3E(H3E), C3F(H3F), C3G(H3G),
 C3H(H3H), C3I(H3I), C3J(H3J), C3K(H3K), C3L(H3L), C3M(H3M), C3N(H3N), C3O(H3O),
  C3P(H3P), C3Q(H3Q), C3R(H3R), C3S(H3S), C3T(H3T), C3U(H3U), C3V(H3V),
 C3W(H3W), C3X(H3X), C3Y(H3Y), C3Z(H3Z), C40(H40), C41(H41), C42(H42), C43(H43),
  C44(H44), C45(H45), C46(H46), C48(H48), C4A(H4A), C4C(H4C), C4D(H4D),
 C4E(H4E), C4F(H4F), C4H(H4H), C4J(H4J), C4K(H4K), C4L(H4L), C4O(H4O), C4Q(H4Q),
  C4R(H4R), C4T(H4T), C4X(H4X), C4Y(H4Y), C51(H51), C58(H58A), C59(H59),
 C5C(H5C), C5D(H5D), C5F(H5F), C5H(H5H), C5I(H5I), C5B(H5B), C33(H33), C57(H57),
  C5K(H5K), C5O(H5O), C4M(H4M), C4V(H4V), C54(H54), C53(H53), C4U(H4U),
 C4N(H4N), C29(H29A), C4I(H4I), C4Z(H4Z), C3D(H3DA)
3.b Fitted hexagon refined as free rotating group:
 C5H(C5I,C5B,C33,C57,C50), C4M(C4V,C54,C53,C4U,C10), C4N(C29,C4I,C4Z,C3D,C4G)
3.c Idealised Me refined as rotating group:
 C83(H83A,H83B,H83C), C3(H3A,H3C,H3D), C1G(H1GA,H1GB,H1GC), C1J(H1JA,H1JB,
 H1JC), C1N(H1NA,H1NB,H1NC), C1U(H1UA,H1UB,H1UC), C2B(H2BA,H2BB,H2BC), C2M(H2MA,
 H2MB,H2MC), C2V(H2VA,H2VB,H2VC), C2X(H2XA,H2XB,H2XC), C47(H47A,H47B,H47C),
 C4B(H4BA,H4BB,H4BC), C4S(H4SA,H4SB,H4SC), C56(H56A,H56B,H56C), C5E(H5EA,H5EB,
 H5EC), C5G(H5GA,H5GB,H5GC), C4P(H4PA,H4PB,H4PC), C52(H52A,H52B,H52C)
;