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_7701372
_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         '2(C58 H96 Ag6.5 N2 O4 Si4), Cl O4'
_chemical_formula_sum            'C116 H192 Ag13 Cl N4 O12 Si8'
_chemical_formula_weight         3497.20
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-08-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-10 deposited with the CCDC.    2019-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                91.328(7)
_cell_angle_beta                 94.827(7)
_cell_angle_gamma                117.772(7)
_cell_formula_units_Z            2
_cell_length_a                   16.217(4)
_cell_length_b                   16.611(4)
_cell_length_c                   29.328(6)
_cell_measurement_reflns_used    9656
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.95
_cell_measurement_theta_min      2.52
_cell_volume                     6948(3)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker SAINT'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0691
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            285113
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         0.698
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.927
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6559
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       plate
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.482
_refine_diff_density_min         -3.609
_refine_diff_density_rms         0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1445
_refine_ls_number_reflns         24428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.1048
_refine_ls_R_factor_gt           0.0864
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0835P)^2^+238.8645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2332
_refine_ls_wR_factor_ref         0.2530
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19963
_reflns_number_total             24428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03697k2.cif
_cod_data_source_block           ag_ag_501_0m_a
_cod_database_code               7701372
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.893
_shelx_estimated_absorpt_t_min   0.723
_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. Others
 Fixed Sof: Ag4(0.5)
3.a Ternary CH refined with riding coordinates:
 C3(H3), C6(H6), C9(H9), C17(H17), C20(H20), C25(H25), C28(H28), C31(H31),
 C36(H36), C39(H39), C42(H42), C61(H61), C64(H64), C67(H67), C72(H72), C75(H75),
  C78(H78), C83(H83), C86(H86), C89(H89), C106(H106), C110(H110), C113(H113),
 C116(H116)
3.b Aromatic/amide H refined with riding coordinates:
 C47(H47), C50(H50), C51(H51), C54(H54), C57(H57), C58(H58), C94(H94),
 C97(H97), C98(H98), C101(H101), C104(H104), C105(H105)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C37(H37A,H37B,H37C), C38(H38A,H38B,
 H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C49(H49A,H49B,H49C), C56(H56A,H56B,H56C), C62(H62A,H62B,H62C),
 C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C68(H68A,H68B,
 H68C), C69(H69A,H69B,H69C), C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C76(H76A,
 H76B,H76C), C77(H77A,H77B,H77C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C),
 C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C87(H87A,H87B,H87C), C88(H88A,H88B,
 H88C), C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C96(H96A,H96B,H96C),
 C103(H10G,H10H,H10I), C107(H10D,H10E,H10F), C111(H11D,H11E,H11F), C112(H11G,
 H11H,H11I), C114(H11J,H11K,H11L), C115(H11M,H11N,H11O), C117(H11P,H11Q,H11R),
 C118(H11S,H11T,H11U)
;
_shelx_res_checksum              63295
_olex2_submission_special_instructions 'No special instructions were received'