A hexaicosametallic copper(ii) phosphonate.
Chandrasekhar, Vadapalli; Sahoo, Dipankar; Narayanan, Ramakirushnan Suriya; Butcher, Raymond J.; Lloret, Franscesc; Pardo, Emilio; Dalton transactions (Cambridge, England : 2003) 42 (2013) 8192–8196; doi:10.1039/c3dt00103b

data_7021368
_publ_section_title
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 A hexaicosametallic copper(ii) phosphonate.
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_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8192
_journal_page_last               8196
_journal_paper_doi               10.1039/c3dt00103b
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C206 H298 Cl6 Cu26 N4 O68 P18'
_chemical_formula_sum            'C206 H298 Cl6 Cu26 N4 O68 P18'
_chemical_formula_weight         6340.68
_chemical_name_common            'Cu26_metal phosphonate'
_chemical_name_systematic
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?
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_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-02-23
_audit_creation_method
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Olex2 1.2
(compiled Dec 5 2012 16:20:19, GUI svn.r4385)
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_cell_angle_alpha                90.00
_cell_angle_beta                 114.353(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   39.396(3)
_cell_length_b                   23.230(3)
_cell_length_c                   39.059(5)
_cell_measurement_reflns_used    6835
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.89
_cell_measurement_theta_min      2.2
_cell_volume                     32565(6)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'Bruker Apex 2'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics
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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.
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_computing_publication_material
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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.
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_computing_structure_refinement
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XH, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
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_computing_structure_solution
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XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
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_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0900
_diffrn_reflns_av_unetI/netI     0.1259
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            86350
_diffrn_reflns_theta_full        25.27
_diffrn_reflns_theta_max         25.27
_diffrn_reflns_theta_min         1.84
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.854
_exptl_absorpt_correction_T_max  0.830
_exptl_absorpt_correction_T_min  0.578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS v.2.10 (Bruker,2003) was used for absorption correction.
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_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             12928
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.572
_refine_diff_density_min         -1.268
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1037
_refine_ls_number_reflns         29483
_refine_ls_number_restraints     475
_refine_ls_restrained_S_all      0.899
_refine_ls_R_factor_all          0.1204
_refine_ls_R_factor_gt           0.0739
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1135P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1903
_refine_ls_wR_factor_ref         0.2114
_reflns_number_gt                14384
_reflns_number_total             29483
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt00103b.txt
_cod_data_source_block           892148
_cod_original_cell_volume        32564(7)
_cod_database_code               7021368
_olex2_refinement_description
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1. Fixed Uiso
At 1.2 times of:
{H1DA,H1DB} of C1D, H5D of C5D, {H1EA,H1EB} of C1E, H5E of C5E, {H1FA,H1FB}
of C1F, H5F of C5F, {H1GA,H1GB} of C1G, H5A of C5A, {H1AA,H1AB} of C1A, {H1CA,
H1CB} of C1C, {H1BA,H1BB} of C1B, H5B of C5B, H5C of C5C, H5I of C5I, H1I of
C1I, {H1HA,H1HB} of C1H, H5G of C5G, H5H of C5H
At 1.5 times of:
{H9DA,H9DB,H9DC} of C9D, {H11J,H11K,H11L} of C11D, {H8DA,H8DB,H8DC} of C8D,
{H10J,H10K,H10L} of C10D, {H11M,H11N,H11O} of C11E, {H9EA,H9EB,H9EC} of C9E,
{H10M,H10N,H10O} of C10E, {H8EA,H8EB,H8EC} of C8E, {H8FA,H8FB,H8FC} of C8F,
{H9FA,H9FB,H9FC} of C9F, {H10P,H10Q,H10R} of C10F, {H11P,H11Q,H11R} of C11F,
{H8AA,H8AB,H8AC} of C8A, {H11A,H11B,H11C} of C11A, {H9AA,H9AB,H9AC} of C9A,
{H10A,H10B,H10C} of C10A, {H8BA,H8BB,H8BC} of C8B, {H10D,H10E,H10F} of C10B,
{H11D,H11E,H11F} of C11B, {H9BA,H9BB,H9BC} of C9B, {H8CA,H8CB,H8CC} of C8C,
{H9CA,H9CB,H9CC} of C9C, {H11G,H11H,H11I} of C11C, {H10G,H10H,H10I} of C10C,
{H8IA,H8IB,H8IC} of C8I, {H10Y,H10Z,H10{} of C10I, {H9IA,H9IB,H9IC} of C9I,
{H11Y,H11Z,H11{} of C11I, H1HY of O1HY, {H2HA,H2HB} of O2HY, H7HY of O7HY,
{H7A,H7B,H7C} of C7, {H3HA,H3HB} of O3HY, H6HY of O6HY, {H22A,H22B,H22C} of
C22S, H5HY of O5HY, H4HY of O4HY, {H8GA,H8GB,H8GC} of C8G, {H11S,H11T,H11U}
of C11G, {H9GA,H9GB,H9GC} of C9G, {H10S,H10T,H10U} of C10G, {H8HA,H8HB,H8HC}
of C8H, {H9HA,H9HB,H9HC} of C9H, {H10V,H10W,H10X} of C10H, {H11V,H11W,H11X}
of C11H
2. Restrained distances
N2S-C22S
2.68 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C8) ~ Ueq, Uanis(C7) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C21S) ~ Ueq, Uanis(C22S) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C9G) ~ Ueq, Uanis(C8G) ~ Ueq, Uanis(C11G) ~ Ueq, Uanis(C10G) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C9G) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C10C) ~ Ueq, Uanis(C6C) ~ Ueq, Uanis(C5C) ~ Ueq, Uanis(C9C) ~ Ueq, Uanis(C4C) ~ Ueq, Uanis(C8C) ~ Ueq, Uanis(C3C) ~ Ueq, Uanis(C7C) ~ Ueq, Uanis(C11C) ~ Ueq, Uanis(C2C) ~ Ueq, Uanis(C1C) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C1F) ~ Ueq, Uanis(C2F) ~ Ueq, Uanis(C3F) ~ Ueq, Uanis(C8F) ~ Ueq, Uanis(C4F) ~ Ueq, Uanis(C9F) ~ Ueq, Uanis(C5F) ~ Ueq, Uanis(C6F) ~ Ueq, Uanis(C7F) ~ Ueq, Uanis(C11F) ~ Ueq, Uanis(C10F) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C1H) ~ Ueq, Uanis(C2H) ~ Ueq, Uanis(C3H) ~ Ueq, Uanis(C8H) ~ Ueq, Uanis(C4H) ~ Ueq, Uanis(C9H) ~ Ueq, Uanis(C5H) ~ Ueq, Uanis(C6H) ~ Ueq, Uanis(C10H) ~ Ueq, Uanis(C7H) ~ Ueq, Uanis(C11H) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C8G) ~ Ueq, Uanis(C3G) ~ Ueq, Uanis(C2G) ~ Ueq, Uanis(C1G) ~ Ueq, Uanis(C7G) ~ Ueq, Uanis(C11G) ~ Ueq, Uanis(C6G) ~ Ueq, Uanis(C5G) ~ Ueq, Uanis(C4G) ~ Ueq, Uanis(C9G) ~ Ueq, Uanis(C10G) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C9A) ~ Ueq, Uanis(C4A) ~ Ueq, Uanis(C5A) ~ Ueq, Uanis(C6A) ~ Ueq, Uanis(C10A) ~ Ueq, Uanis(C7A) ~ Ueq, Uanis(C11A) ~ Ueq, Uanis(C2A) ~ Ueq, Uanis(C3A) ~ Ueq, Uanis(C8A) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
Uanis(C3A) ~ Ueq, Uanis(C4A) ~ Ueq, Uanis(C5A) ~ Ueq, Uanis(C6A) ~ Ueq, Uanis(C7A) ~ Ueq, Uanis(C2A) ~ Ueq, Uanis(C8A) ~ Ueq, Uanis(C9A) ~ Ueq, Uanis(C10A) ~ Ueq, Uanis(C11A) ~ Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C2H) ~ Ueq, Uanis(C7H) ~ Ueq, Uanis(C6H) ~ Ueq, Uanis(C5H) ~ Ueq, Uanis(C4H) ~ Ueq, Uanis(C3H) ~ Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C8) = Uanis(C7)
Uanis(C9G) = Uanis(C8G) = Uanis(C11G) = Uanis(C10G)
Uanis(C21S) = Uanis(C22S)
Uanis(C9B) = Uanis(C8B) = Uanis(C10B) = Uanis(C11B) = Uanis(C1B) = Uanis(C2B) = Uanis(C3B) = Uanis(C4B) = Uanis(C5B) = Uanis(C7B) = Uanis(C6B)
Uanis(C9E) = Uanis(C4E) = Uanis(C8E) = Uanis(C5E) = Uanis(C3E) = Uanis(C2E) = Uanis(C7E) = Uanis(C6E) = Uanis(C10E) = Uanis(C11E) = Uanis(C1E)
Uanis(C1C) = Uanis(C7C) = Uanis(C11C) = Uanis(C2C) = Uanis(C8C) = Uanis(C3C) = Uanis(C4C) = Uanis(C9C) = Uanis(C5C) = Uanis(C6C) = Uanis(C10C)
Uanis(C8F) = Uanis(C3F) = Uanis(C4F) = Uanis(C1F) = Uanis(C2F) = Uanis(C7F) = Uanis(C11F) = Uanis(C6F) = Uanis(C10F) = Uanis(C5F) = Uanis(C9F)
Uanis(C1H) = Uanis(C11H) = Uanis(C7H) = Uanis(C2H) = Uanis(C3H) = Uanis(C4H) = Uanis(C5H) = Uanis(C6H) = Uanis(C10H) = Uanis(C9H) = Uanis(C8H)
Uanis(C11I) = Uanis(C7I) = Uanis(C6I) = Uanis(C10I) = Uanis(C5I) = Uanis(C4I) = Uanis(C9I) = Uanis(C8I) = Uanis(C3I) = Uanis(C2I) = Uanis(C1I)
Uanis(C4A) = Uanis(C5A) = Uanis(C6A) = Uanis(C7A) = Uanis(C2A) = Uanis(C3A) = Uanis(C8A) = Uanis(C9A) = Uanis(C10A) = Uanis(C11A)
4.a Riding coordinates:
O1HY(H1HY), O5HY(H5HY), O6HY(H6HY), O7HY(H7HY)
4.b Rotating group:
O2HY(H2HA,H2HB)
4.c Ternary CH refined with riding coordinates:
O4HY(H4HY)
4.d Secondary CH2 refined with riding coordinates:
C1A(H1AA,H1AB), C1B(H1BA,H1BB), C1C(H1CA,H1CB), C1D(H1DA,H1DB), C1E(H1EA,
H1EB), C1F(H1FA,H1FB), C1G(H1GA,H1GB), C1H(H1HA,H1HB), O3HY(H3HA,H3HB)
4.e Me refined with riding coordinates:
C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C10A(H10A,H10B,H10C), C11A(H11A,
H11B,H11C), C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,H10F),
C11B(H11D,H11E,H11F), C8C(H8CA,H8CB,H8CC), C9C(H9CA,H9CB,H9CC), C10C(H10G,H10H,
H10I), C11C(H11G,H11H,H11I), C8D(H8DA,H8DB,H8DC), C9D(H9DA,H9DB,H9DC),
C11D(H11J,H11K,H11L), C8E(H8EA,H8EB,H8EC), C9E(H9EA,H9EB,H9EC), C11E(H11M,H11N,
H11O), C8F(H8FA,H8FB,H8FC), C9F(H9FA,H9FB,H9FC), C10F(H10P,H10Q,H10R),
C11F(H11P,H11Q,H11R), C8G(H8GA,H8GB,H8GC), C9G(H9GA,H9GB,H9GC), C10G(H10S,H10T,
H10U), C11G(H11S,H11T,H11U), C8H(H8HA,H8HB,H8HC), C9H(H9HA,H9HB,H9HC),
C10H(H10V,H10W,H10X), C11H(H11V,H11W,H11X), C8I(H8IA,H8IB,H8IC), C9I(H9IA,H9IB,
H9IC), C10I(H10Y,H10Z,H10{), C11I(H11Y,H11Z,H11{), C22S(H22A,H22B,H22C)
4.f Aromatic/amide H refined with riding coordinates:
C5A(H5A), C5B(H5B), C5C(H5C), C5D(H5D), C5E(H5E), C5F(H5F), C5G(H5G),
C5H(H5H), C1I(H1I), C5I(H5I)
4.g Idealised Me refined as rotating group:
C10D(H10J,H10K,H10L), C10E(H10M,H10N,H10O), C7(H7A,H7B,H7C)
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