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_7701369
_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         'C62 H68 Ag10 N3 O12 S6, 3(Cl O4)'
_chemical_formula_sum            'C62 H68 Ag10 Cl3 N3 O24 S6'
_chemical_formula_weight         2616.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-03-06
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.489(3)
_cell_length_b                   18.767(4)
_cell_length_c                   25.470(5)
_cell_measurement_reflns_used    7834
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      20.88
_cell_measurement_theta_min      2.17
_cell_volume                     7882(3)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123.15
_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  0.2043
_diffrn_reflns_av_unetI/netI     0.1225
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            96189
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.348
_exptl_absorpt_coefficient_mu    2.762
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.205
_exptl_crystal_description       rod
_exptl_crystal_F_000             5080
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.527
_refine_diff_density_min         -1.958
_refine_diff_density_rms         0.275
_refine_ls_abs_structure_details
;
 Flack x determined using 3301 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.10(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     987
_refine_ls_number_reflns         13905
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1226
_refine_ls_R_factor_gt           0.0730
_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^)+(0.0784P)^2^+85.9333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1636
_refine_ls_wR_factor_ref         0.1893
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9661
_reflns_number_total             13905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03697k2.cif
_cod_data_source_block           ag_ag_200_0m_a
_cod_database_code               7701369
_shelx_shelxl_version_number     2014/7
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 S2S-C3S = S2S-C4S
 1.78 with sigma of 0.02
 S2S-C3S \\sim S2S-C4S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C11) \\sim
Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(C49) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C34)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C3S) \\sim Ueq, Uanis(C4S) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C3S) = Uanis(C4S)
4. Others
 Sof(H3SD)=Sof(H3SE)=Sof(H3SF)=Sof(H4SD)=Sof(H4SE)=Sof(H4SF)=Sof(S2T)=1-FVAR(1)
 Sof(H3SA)=Sof(H3SB)=Sof(H3SC)=Sof(H4SA)=Sof(H4SB)=Sof(H4SC)=Sof(S2S)=FVAR(1)
5.a Me refined with riding coordinates:
 C3S(H3SA,H3SB,H3SC), C3S(H3SD,H3SE,H3SF), C4S(H4SA,H4SB,H4SC), C4S(H4SD,H4SE,
 H4SF)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C28(H28),
  C29(H29), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36), C37(H37),
 C38(H38), C41(H41), C42(H42), C43(H43), C44(H44), C47(H47), C48(H48), C49(H49),
  C50(H50)
5.c Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC), C5S(H5SA,H5SB,H5SC), C6S(H6SA,H6SB,
 H6SC), C7S(H7SA,H7SB,H7SC), C8S(H8SA,H8SB,H8SC), C9S(H9SA,H9SB,H9SC),
 C10S(H10A,H10B,H10C), C11S(H11A,H11B,H11C), C12S(H12A,H12B,H12C)
;
_shelx_res_checksum              59031
_olex2_submission_special_instructions 'No special instructions were received'