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_7701368
_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         'C38 H50 Ag7 N2 O5, C F3 O3 S'
_chemical_formula_sum            'C39 H50 Ag7 F3 N2 O8 S'
_chemical_formula_weight         1518.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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            16
_cell_length_a                   38.814(6)
_cell_length_b                   53.264(8)
_cell_length_c                   9.9806(15)
_cell_measurement_reflns_used    7081
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.80
_cell_measurement_theta_min      2.23
_cell_volume                     20634(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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0880
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       63
_diffrn_reflns_limit_k_min       -63
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            41137
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.246
_diffrn_reflns_theta_min         1.529
_exptl_absorpt_coefficient_mu    2.697
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.956
_exptl_crystal_description       plate
_exptl_crystal_F_000             11744
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.382
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.207
_refine_ls_abs_structure_details
;
 Flack x determined using 2565 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         8717
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0645
_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^)+(0.0395P)^2^+944.1216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1321
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    0.861
_reflns_Friedel_fraction_max     0.860
_reflns_number_gt                7437
_reflns_number_total             8717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03697k2.cif
_cod_data_source_block           1_a
_cod_database_code               7701368
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O1S-C1S
 1.33 with sigma of 0.02
 C1S-C2S
 1.45 with sigma of 0.02
 O1S-H1S
 1.1 with sigma of 0.02
 S1-O1A \\sim S1-O2A \\sim S1-O3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C7C) \\sim Ueq, Uanis(C24)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C9) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
4.b Aromatic/amide H refined with riding coordinates:
 C1C(H1C), C2C(H2C), C3C(H3C), C4C(H4CA), C9C(H9C), C10C(H10D), C11C(H11D),
 C12C(H12D)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C2S(H2SA,H2SB,H2SC)
;
_shelx_res_checksum              69643
_olex2_submission_special_instructions 'No special instructions were received'