Molecular and polymeric zinc(ii) phosphonates: isolation of an octanuclear ellipsoidal ensemble.
Sahoo, Dipankar; Suriyanarayanan, Ramakirushnan; Metre, Ramesh K; Chandrasekhar, Vadapalli; Dalton transactions (Cambridge, England : 2003) 43 (2014) 7304–7313; doi:10.1039/c3dt53614a

data_7029852
_publ_section_title
;
 Molecular and polymeric zinc(ii) phosphonates: isolation of an
 octanuclear ellipsoidal ensemble.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7304
_journal_page_last               7313
_journal_paper_doi               10.1039/c3dt53614a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety
'C78 H120 Cl6 N2 O18 P6 Zn8, C78 H119 Cl6 N2 O18 P6 Zn8, 2(C6 H16 N), 2(C6 H15 N), 1.5(H2 O), H2 O0.5'
_chemical_formula_sum            'C180 H306 Cl12 N8 O38 P12 Zn16'
_chemical_formula_weight         5033.27
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-02-17
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                93.974(2)
_cell_angle_beta                 92.518(2)
_cell_angle_gamma                91.439(2)
_cell_formula_units_Z            2
_cell_length_a                   14.1126(12)
_cell_length_b                   26.267(2)
_cell_length_c                   33.873(3)
_cell_measurement_reflns_used    8379
_cell_measurement_temperature    100(2)
_cell_volume                     12509.3(18)
_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-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.984
_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  0.0462
_diffrn_reflns_av_unetI/netI     0.1359
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            74382
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         0.777
_exptl_absorpt_coefficient_mu    1.766
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.087374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0817 before and 0.0325 after correction.
The Ratio of minimum to maximum transmission is 0.0874.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       block
_exptl_crystal_F_000             5220
_exptl_crystal_size_max          0.096
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.848
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2426
_refine_ls_number_reflns         45793
_refine_ls_number_restraints     304
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.1673
_refine_ls_R_factor_gt           0.0878
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1531P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2272
_refine_ls_wR_factor_ref         0.2738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21016
_reflns_number_total             45793
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt53614a2.cif
_cod_data_source_block           978376
_cod_depositor_comments
;Adding full bibliography for
 ./tmp-cod-update-bibliographies-12899/cifs/7029852.cif.
;
_cod_database_code               7029852
_shelxl_version_number           2013-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups, All O(H,H,H,H) groups
2. Restrained distances
 C1A-C89S
 1.54 with sigma of 0.02
 C88-C87
 1.54 with sigma of 0.02
 C85-C86
 1.54 with sigma of 0.02
 C85-C86
 1.54 with sigma of 0.02
 C89S-C1A
 1.54 with sigma of 0.02
 C85S-C86S
 1.54 with sigma of 0.02
 C87S-C88S
 1.54 with sigma of 0.02
 N6S-C85S
 1.4 with sigma of 0.02
 N6S-C89S
 1.4 with sigma of 0.02
 N6S-C87S
 1.4 with sigma of 0.02
 C88S-C87S
 1.54 with sigma of 0.02
 C85S-C86S
 1.54 with sigma of 0.02
 H1BB-O1B
 0.82 with sigma of 0.02
 H1BA-O1B
 0.82 with sigma of 0.02
 C87S-C89S
 2.3 with sigma of 0.04
 H1BA-H1BB
 1.3 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C83S) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C89S) \\sim Ueq, Uanis(C87S) \\sim Ueq, Uanis(C88S) \\sim Ueq,
Uanis(C85S) \\sim Ueq, Uanis(C86S) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C79) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C81S) \\sim Ueq, Uanis(C82S)
\\sim Ueq, Uanis(C80S) \\sim Ueq, Uanis(C79S) \\sim Ueq: with sigma of 0.001
and sigma for terminal atoms of 0.002
Uanis(N6S) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C48S) \\sim Ueq, Uanis(C49S) \\sim Ueq, Uanis(C47S) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C53S) \\sim Ueq, Uanis(C54S) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C73S) \\sim Ueq, Uanis(C75S) \\sim Ueq, Uanis(C77S) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C88) \\sim Ueq, Uanis(C87) \\sim Ueq: with sigma of 0.0007 and sigma for
terminal atoms of 0.002
Uanis(C1A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C21S) \\sim Ueq, Uanis(C20S) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C32S) \\sim Ueq, Uanis(C31S) \\sim Ueq, Uanis(C25S) \\sim Ueq,
Uanis(C26S) \\sim Ueq, Uanis(C27S) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C22) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C17) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C67) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C72) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C89) \\sim Ueq, Uanis(C90) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C85) \\sim Ueq, Uanis(C86) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C87) \\sim Ueq, Uanis(C88) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C31S) \\sim Ueq, Uanis(C32S) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C77)
\\sim Ueq, Uanis(C64S) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(C85S) = Uanis(C89S)
Uanis(C85S) = Uanis(C86S)
Uanis(C87S) = Uanis(C88S)
Uanis(C79S) = Uanis(C80S)
Uanis(C83S) = Uanis(C84S)
Uanis(C79) = Uanis(C80)
Uanis(C81) = Uanis(C82)
Uanis(C85) = Uanis(C86)
Uanis(C87) = Uanis(C88)
Uanis(C89) = Uanis(C90)
4. Others
 Fixed Sof: O19(0.5) H19G(0.5) H19H(0.5) O1A(0.5) H1AD(0.5) H1AE(0.5) O1B(0.5)
 O1C(0.5) H1CA(0.5) H1CB(0.5)
5.a Riding coordinates:
 N5(H5), N6(H6), N5S(H5S), C80(H80A,H80B,H80C), C86(H86A,H86B,H86C), C88(H88A,
 H88B,H88C), C84S(H84D,H84E,H84F), C88S(H88D,H88E,H88F), O19(H19G,H19H),
 O1A(H1AD,H1AE), O1C(H1CA,H1CB)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C18(H18A,H18B), C29(H29A,H29B), C40(H40A,H40B), C51(H51A,H51B),
 C62(H62A,H62B), C67(H67A,H67B), C69(H69A,H69B), C71(H71A,H71B), C73(H73A,H73B),
  C75(H75A,H75B), C77(H77A,H77B), C79(H79A,H79B), C81(H81A,H81B), C83(H83A,
 H83B), C85(H85A,H85B), C87(H87A,H87B), C89(H89A,H89B), C7S(H7SA,H7SB),
 C18S(H18C,H18D), C29S(H29C,H29D), C40S(H40C,H40D), C62S(H62C,H62D), C67S(H67C,
 H67D), C69S(H69C,H69D), C71S(H71C,H71D), C73S(H73C,H73D), C75S(H75C,H75D),
 C77S(H77C,H77D), C81S(H81C,H81D), C83S(H83C,H83D), C85S(H85C,H85D), C87S(H87C,
 H87D), C89S(H89C,H89D)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C15(H15), C26(H26), C37(H37), C48(H48), C59(H59), C4S(H4S),
 C15S(H15S), C26S(H26S), C37S(H37S), C48S(H48S), C51S(H51S), C59S(H59S),
 C79S(H79S)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,
 H54C), C55(H55A,H55B,H55C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,
 H65B,H65C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C),
 C72(H72A,H72B,H72C), C74(H74A,H74B,H74C), C76(H76A,H76B,H76C), C78(H78A,H78B,
 H78C), C82(H82A,H82B,H82C), C84(H84A,H84B,H84C), C90(H90A,H90B,H90C), C8S(H8SA,
 H8SB,H8SC), C9S(H9SA,H9SB,H9SC), C10S(H10D,H10E,H10F), C11S(H11D,H11E,H11F),
 C19S(H19D,H19E,H19F), C20S(H20D,H20E,H20F), C21S(H21D,H21E,H21F), C22S(H22D,
 H22E,H22F), C30S(H30D,H30E,H30F), C31S(H31D,H31E,H31F), C32S(H32D,H32E,H32F),
 C33S(H33D,H33E,H33F), C41S(H41D,H41E,H41F), C42S(H42D,H42E,H42F), C43S(H43D,
 H43E,H43F), C44S(H44D,H44E,H44F), C52S(H52D,H52E,H52F), C53S(H53D,H53E,H53F),
 C54S(H54D,H54E,H54F), C55S(H55D,H55E,H55F), C63S(H63D,H63E,H63F), C64S(H64D,
 H64E,H64F), C65S(H65D,H65E,H65F), C66S(H66D,H66E,H66F), C68S(H68D,H68E,H68F),
 C70S(H70D,H70E,H70F), C72S(H72D,H72E,H72F), C74S(H74D,H74E,H74F), C76S(H76D,
 H76E,H76F), C78S(H78D,H78E,H78F), C80S(H80D,H80E,H80F), C82S(H82D,H82E,H82F),
 C86S(H86D,H86E,H86F), C1A(H1AA,H1AB,H1AC)
;