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_7701367
_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         'C16 H18 Ag4 Cl0.5 N O4, 0.5(Cl O4)'
_chemical_formula_sum            'C16 H18 Ag4 Cl N O6'
_chemical_formula_weight         787.24
_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             2019-08-28
_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                90
_cell_angle_beta                 126.986(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.465(6)
_cell_length_b                   24.276(9)
_cell_length_c                   13.433(5)
_cell_measurement_reflns_used    3133
_cell_measurement_temperature    150
_cell_measurement_theta_max      22.05
_cell_measurement_theta_min      2.53
_cell_volume                     4289(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
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruke ApexII with microsource'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1244
_diffrn_reflns_av_unetI/netI     0.0818
_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       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27979
_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         1.678
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.755
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.3966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_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    2.438
_exptl_crystal_description       needle
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.357
_refine_diff_density_min         -2.034
_refine_diff_density_rms         0.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         3773
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0773P)^2^+117.1800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1460
_refine_ls_wR_factor_ref         0.1711
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2501
_reflns_number_total             3773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03697k2.cif
_cod_data_source_block           ag_ag_504_0m_a
_cod_database_code               7701367
_shelx_shelxl_version_number     2018/3
_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
 Cl1_1-O1_1 = Cl1_1-O2_1 = Cl1_1-O3_1 = Cl1_1-O4_1
 1.501 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3C) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O1_1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O1C) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 Cl1_1, O1_1, O2_1, O3_1, O4_1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15, C14, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, O4C, O3C, O2C, O1C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cl1(0.5) O1C(0.5) O2C(0.5) O3C(0.5) O4C(0.5) Cl1(0.5) O1(0.5)
 O2(0.5) O3(0.5) O4(0.5)
6.a Ternary CH refined with riding coordinates:
 C9(H9), C14(H14)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6)
6.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C)
;
_shelx_res_checksum              55848
_olex2_submission_special_instructions 'No special instructions were received'