Facile synthesis of silver alkynide cluster and coordination polymers using picolinic acid as co-ligand
Gupta, Arvind Kumar Kumar; Orthaber, Andreas; Dalton Transactions  (2019) –; doi:10.1039/C9DT03697K

data_7701366
_publ_section_title
;
 Facile synthesis of silver alkynide cluster and coordination polymers
 using picolinic acid as co-ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03697K
_journal_year                    2019
_chemical_formula_moiety         'C112 H184 Ag13 N4 O8 Si8, Cl O4'
_chemical_formula_sum            'C112 H184 Ag13 Cl N4 O12 Si8'
_chemical_formula_weight         3441.10
_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     dual
_audit_creation_date             2019-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-11 deposited with the CCDC.    2019-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.7990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.1488(6)
_cell_length_b                   16.3089(4)
_cell_length_c                   28.5179(6)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.52
_cell_volume                     13550.3(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            56034
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.007
_exptl_absorpt_coefficient_mu    1.975
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_description       Prism
_exptl_crystal_F_000             6880
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         11916
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+63.2492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9652
_reflns_number_total             11916
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03697k2.cif
_cod_data_source_block           ag_ag_85_0m_a
_cod_database_code               7701366
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C81-C82 = C81-C83
 1.58 with sigma of 0.02
 Si3-C81 \\sim Si3-C81A
 with sigma of 0.02
 C81-C82 \\sim C81A-C82A
 with sigma of 0.02
 C81-C83 \\sim C81A-C83A
 with sigma of 0.02
 Si3-C82 \\sim Si3-C82A
 with sigma of 0.04
 Si3-C83 \\sim Si3-C83A
 with sigma of 0.04
 C82-C83 \\sim C82A-C83A
 with sigma of 0.04
 Cl2-O5 \\sim Cl2-O6 \\sim Cl2-O7 \\sim Cl2-O8
 with sigma of 0.02
 O5-O7 \\sim O6-O8 \\sim O5-O8 \\sim O6-O7 \\sim O5-O6 \\sim O7-O8
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Cl2 \\sim O5 \\sim O6 \\sim O7 \\sim O8: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C82) \\sim Ueq, Uanis(C83) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(O6) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim
Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.06
4. Rigid body (RIGU) restrains
 Cl2, O5, O6, O7, O8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, Cl2, O5, O7, O8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C82A)=Sof(H82D)=Sof(H82E)=Sof(H82F)=Sof(C81A)=Sof(H81A)=Sof(C83A)=
 Sof(H83D)=Sof(H83E)=Sof(H83F)=1-FVAR(1)
 Sof(C81)=Sof(H81)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(H82C)=Sof(C83)=Sof(H83A)=
 Sof(H83B)=Sof(H83C)=FVAR(1)
 Fixed Sof: Cl2(0.5) O5(0.5) O6(0.5) O7(0.5) O8(0.5)
6.a Ternary CH refined with riding coordinates:
 C11(H11), C21(H21), C31(H31), C41(H41), C51(H51), C61(H61), C71(H71),
 C81(H81), C91(H91), C101(H101), C111(H111), C121(H121), C81A(H81A)
6.b Aromatic/amide H refined with riding coordinates:
 C3L(H3L), C4L(H4L), C5L(H5L), C6L(H6L), C9L(H9L), C10L(H10L), C11L(H11L),
 C12L(H12L)
6.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C62(H62A,H62B,H62C),
 C63(H63A,H63B,H63C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C92(H92A,H92B,
 H92C), C93(H93A,H93B,H93C), C102(H10A,H10B,H10C), C103(H10D,H10E,H10F),
 C112(H11A,H11B,H11C), C113(H11D,H11E,H11F), C122(H12D,H12E,H12F), C123(H12G,
 H12H,H12I), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C82A(H82D,H82E,H82F),
 C83A(H83D,H83E,H83F)
;
_shelx_res_checksum              84675
_olex2_submission_special_instructions 'No special instructions were received'