Lipophilic bismuth phosphates: a molecular tetradecanuclear cage and a 1D-coordination polymer. Synthesis, structure and conversion to BiPO4.
Chandrasekhar, Vadapalli; Metre, Ramesh K.; Suriya Narayanan, Ramakirushnan; Dalton transactions (Cambridge, England : 2003) 42 (2013) 8709–8716; doi:10.1039/c3dt50537e

data_7023027
_publ_section_title
;
 Lipophilic bismuth phosphates: a molecular tetradecanuclear cage and a
 1D-coordination polymer. Synthesis, structure and conversion to BiPO4.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8709
_journal_page_last               8716
_journal_paper_doi               10.1039/c3dt50537e
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C146 H214 Bi14 O60 P12'
_chemical_formula_sum            'C146 H214 Bi14 O60 P12'
_chemical_formula_weight         6226.53
_chemical_name_systematic
;
?
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-02-26
_audit_creation_method
;
Olex2 1.2
(compiled Dec 5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                113.340(5)
_cell_angle_beta                 97.276(5)
_cell_angle_gamma                107.712(5)
_cell_formula_units_Z            1
_cell_length_a                   17.775(5)
_cell_length_b                   18.252(5)
_cell_length_c                   19.813(5)
_cell_measurement_reflns_used    4633
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.48
_cell_measurement_theta_min      2.44
_cell_volume                     5393(3)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XH, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.981
_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  0.0579
_diffrn_reflns_av_unetI/netI     0.1594
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34446
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.67
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    11.524
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.435509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.1098 before and 0.0392 after correction.
The Ratio of minimum to maximum transmission is 0.4355.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         3.144
_refine_diff_density_min         -2.008
_refine_diff_density_rms         0.331
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     590
_refine_ls_number_reflns         19680
_refine_ls_number_restraints     556
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.1180
_refine_ls_R_factor_gt           0.0729
_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^)+(0.1083P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1778
_refine_ls_wR_factor_ref         0.1996
_reflns_number_gt                11423
_reflns_number_total             19680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50537e.txt
_cod_data_source_block           1
_cod_database_code               7023027
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
H7 of C7, H22 of C22, H13 of C13, H10 of C10, H9 of C9, H20 of C20, {H33A,
H33B} of C33, H35 of C35, H32 of C32, H29 of C29, H31 of C31, H24 of C24, H25
of C25, H3 of C3, H64 of C64, H63 of C63, {H77A,H77B} of C77, H146 of C146,
H147 of C147, H145 of C145, H38 of C38, H45 of C45, H44 of C44, H41 of C41,
H53 of C53, H54 of C54, H42 of C42, H48 of C48, H52 of C52, H46 of C46
At 1.5 times of:
{H37A,H37B,H37C} of C37, {H36A,H36B,H36C} of C36, {H14A,H14B,H14C} of C14,
{H15A,H15B,H15C} of C15, {H4A,H4B,H4C} of C4, {H23A,H23B,H23C} of C23, {H30A,
H30B,H30C} of C30, {H67A,H67B,H67C} of C67, {H60A,H60B,H60C} of C60, {H62A,
H62B,H62C} of C62, {H65A,H65B,H65C} of C65, {H59A,H59B,H59C} of C59, {H61A,
H61B,H61C} of C61, {H66A,H66B,H66C} of C66, {H71A,H71B,H71C} of C71, {H78A,
H78B,H78C} of C78, {H72A,H72B,H72C} of C72, {H73A,H73B,H73C} of C73, {H74A,
H74B,H74C} of C74, {H80A,H80B,H80C} of C80, {H70A,H70B,H70C} of C70, {H81A,
H81B,H81C} of C81, {H47A,H47B,H47C} of C47, {H51A,H51B,H51C} of C51, {H55A,
H55B,H55C} of C55
2. Restrained distances
C63-C74 = C63-C78 = C63-C56
1.54 with sigma of 0.02
C64-C65 = C64-C80 = C64-C40
1.54 with sigma of 0.02
C38-C16 = C38-C62 = C38-C73
1.54 with sigma of 0.02
C13-C12 = C13-C14
1.54 with sigma of 0.02
C13-C15
1.54 with sigma of 0.02
C29-C28 = C29-C30 = C29-C59
1.54 with sigma of 0.02
C35-C34 = C35-C36 = C35-C37
1.54 with sigma of 0.02
C22-C21 = C22-C23 = C22-C47
1.54 with sigma of 0.02
C20-C19 = C20-C55 = C20-C66
1.54 with sigma of 0.02
C44-C43 = C44-C71 = C44-C72
1.54 with sigma of 0.02
C3-C4 = C3-C2 = C3-C51
1.54 with sigma of 0.02
C9-C8 = C9-C67 = C9-C70
1.54 with sigma of 0.02
C42-C6 = C42-C60 = C42-C61
1.54 with sigma of 0.02
C13-C15
1.54 with sigma of 0.02
C81-O31
1.4 with sigma of 0.02
C62-C16
2.2 with sigma of 0.04
3. Rigid bond restraints
O31, C81
with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C73) ~ Ueq, Uanis(C62) ~ Ueq, Uanis(C38) ~ Ueq, Uanis(C16) ~ Ueq, Uanis(C77) ~ Ueq, Uanis(C54) ~ Ueq, Uanis(C46) ~ Ueq, Uanis(C12) ~ Ueq, Uanis(C11) ~ Ueq, Uanis(C13) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(O2) ~ Ueq, Uanis(C26) ~ Ueq, Uanis(C145) ~ Ueq, Uanis(C147) ~ Ueq, Uanis(C74) ~ Ueq, Uanis(C63) ~ Ueq, Uanis(C78) ~ Ueq, Uanis(C64) ~ Ueq, Uanis(C80) ~ Ueq, Uanis(C65) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C27) ~ Ueq, Uanis(C28) ~ Ueq, Uanis(C31) ~ Ueq, Uanis(C32) ~ Ueq, Uanis(C33) ~ Ueq, Uanis(C34) ~ Ueq, Uanis(C59) ~ Ueq, Uanis(C29) ~ Ueq, Uanis(C30) ~ Ueq, Uanis(C37) ~ Ueq, Uanis(C35) ~ Ueq, Uanis(C36) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C18) ~ Ueq, Uanis(C19) ~ Ueq, Uanis(C48) ~ Ueq, Uanis(C25) ~ Ueq, Uanis(C24) ~ Ueq, Uanis(C21) ~ Ueq, Uanis(C66) ~ Ueq, Uanis(C55) ~ Ueq, Uanis(C20) ~ Ueq, Uanis(C47) ~ Ueq, Uanis(C22) ~ Ueq, Uanis(C23) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C4) ~ Ueq, Uanis(C51) ~ Ueq, Uanis(C3) ~ Ueq, Uanis(C2) ~ Ueq, Uanis(C45) ~ Ueq, Uanis(C52) ~ Ueq, Uanis(C53) ~ Ueq, Uanis(C43) ~ Ueq, Uanis(C1) ~ Ueq, Uanis(C44) ~ Ueq, Uanis(C72) ~ Ueq, Uanis(C71) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C60) ~ Ueq, Uanis(C42) ~ Ueq, Uanis(C61) ~ Ueq, Uanis(C67) ~ Ueq, Uanis(C70) ~ Ueq, Uanis(C9) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(O14) ~ Ueq, Uanis(O29) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(O14) ~ Ueq, Uanis(O29) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(O29) ~ Ueq, Uanis(O14) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C6) ~ Ueq, Uanis(C7) ~ Ueq, Uanis(C41) ~ Ueq, Uanis(C10) ~ Ueq, Uanis(C8) ~ Ueq, Uanis(C5) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O32) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C81) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O24) ~ Ueq, Uanis(O11) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C146) ~ Ueq, Uanis(C56) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C40) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O34) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C14) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O34) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6) ~ Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C11) = Uanis(C16) = Uanis(C77) = Uanis(C54) = Uanis(C46) = Uanis(C12) = Uanis(C13) = Uanis(C62) = Uanis(C38) = Uanis(C73)
Uanis(C26) = Uanis(C145) = Uanis(C147) = Uanis(C74) = Uanis(C63) = Uanis(C78) = Uanis(C64) = Uanis(C80) = Uanis(C65) = Uanis(C146) = Uanis(C56) = Uanis(C40)
Uanis(C27) = Uanis(C28) = Uanis(C31) = Uanis(C32) = Uanis(C33) = Uanis(C34) = Uanis(C59) = Uanis(C29) = Uanis(C30) = Uanis(C37) = Uanis(C35) = Uanis(C36)
Uanis(C18) = Uanis(C19) = Uanis(C48) = Uanis(C25) = Uanis(C24) = Uanis(C21) = Uanis(C66) = Uanis(C55) = Uanis(C20) = Uanis(C47) = Uanis(C22) = Uanis(C23)
Uanis(C4) = Uanis(C51) = Uanis(C3) = Uanis(C2) = Uanis(C45) = Uanis(C52) = Uanis(C53) = Uanis(C43) = Uanis(C1) = Uanis(C44) = Uanis(C72) = Uanis(C71)
Uanis(C60) = Uanis(C42) = Uanis(C61) = Uanis(C67) = Uanis(C70) = Uanis(C9)
Uanis(O6) = Uanis(O7) = Uanis(O21) = Uanis(O2) = Uanis(O1) = Uanis(O25) = Uanis(O24) = Uanis(O23) = Uanis(O8) = Uanis(O12) = Uanis(O22) = Uanis(O15) = Uanis(O14) = Uanis(O18) = Uanis(O16) = Uanis(O19) = Uanis(O17) = Uanis(O11) = Uanis(O20) = Uanis(O9) = Uanis(O10)
5.a Ternary CH refined with riding coordinates:
C3(H3), C9(H9), C13(H13), C20(H20), C22(H22), C29(H29), C35(H35), C38(H38),
C42(H42), C44(H44), C63(H63), C64(H64)
5.b Secondary CH2 refined with riding coordinates:
C33(H33A,H33B), C77(H77A,H77B)
5.c Aromatic/amide H refined with riding coordinates:
C7(H7), C10(H10), C24(H24), C25(H25), C31(H31), C32(H32), C41(H41), C45(H45),
C46(H46), C48(H48), C52(H52), C53(H53), C54(H54), C146(H146), C145(H145),
C147(H147)
5.d Fitted hexagon refined as free rotating group:
C146(C56,C26,C40,C145,C147)
5.e Idealised Me refined as rotating group:
C4(H4A,H4B,H4C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C23(H23A,H23B,
H23C), C30(H30A,H30B,H30C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C47(H47A,
H47B,H47C), C51(H51A,H51B,H51C), C55(H55A,H55B,H55C), C59(H59A,H59B,H59C),
C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C65(H65A,H65B,
H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C70(H70A,H70B,H70C), C71(H71A,
H71B,H71C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C),
C78(H78A,H78B,H78C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C)
;