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_7029850
_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         'C32 H50 Cl6 N12 O8 P2 Zn4, 2(Cl O4)'
_chemical_formula_sum            'C32 H50 Cl8 N12 O16 P2 Zn4'
_chemical_formula_weight         1465.86
_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             2014-02-18
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                77.438(5)
_cell_angle_beta                 72.645(5)
_cell_angle_gamma                77.177(5)
_cell_formula_units_Z            1
_cell_length_a                   9.998(5)
_cell_length_b                   11.016(5)
_cell_length_c                   13.645(5)
_cell_measurement_reflns_used    1239
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.87
_cell_measurement_theta_min      2.28
_cell_volume                     1380.0(11)
_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 0.982
_diffrn_measured_fraction_theta_max 0.891
_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  0.0424
_diffrn_reflns_av_unetI/netI     0.0986
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8806
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.313
_diffrn_reflns_theta_min         1.585
_exptl_absorpt_coefficient_mu    2.235
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.636984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0758 before and 0.0301 after correction.
The Ratio of minimum to maximum transmission is 0.6370.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_description       block
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.036
_refine_diff_density_max         1.268
_refine_diff_density_min         -1.814
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6134
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1260
_refine_ls_R_factor_gt           0.0693
_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^)+(0.0339P)^2^+19.6994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1332
_refine_ls_wR_factor_ref         0.1972
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3953
_reflns_number_total             6134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt53614a2.cif
_cod_data_source_block           978374
_cod_depositor_comments
;Adding full bibliography for
 ./tmp-cod-update-bibliographies-12899/cifs/7029850.cif.
;
_cod_database_code               7029850
_shelxl_version_number           2013-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H2 of N2, H4A of N4, H6 of N6
 At 1.5 times of:
  All C(H,H,H) groups, H4 of N1
2. Restrained distances
 H4-O4
 0.83 with sigma of 0.02
 H4-Zn2
 2.1 with sigma of 0.04
 H4-Zn2
 2.2 with sigma of 0.04
 Zn1-H4
 2.2 with sigma of 0.04
3.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4A), N6(H6), C3(H3), C8(H8), C13(H13)
3.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;