Assembly of high-symmetry silver(I) alkyl-1,3-diynyl cluster complexes via core transformation
Hau, Sam Chunkit; Mak, Thomas C. W.; Dalton Trans.  (2017) –; doi:10.1039/C7DT03406G

data_7044368
_publ_section_title
;
 Assembly of high-symmetry silver(I) alkyl-1,3-diynyl cluster complexes
 via core transformation
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03406G
_journal_year                    2017
_chemical_formula_moiety         'C186 H148 Ag8 P8, 2(N O3), 2(O)'
_chemical_formula_sum            'C187 H153 Ag8 N2 O8 P8'
_chemical_formula_weight         3666.82
_chemical_name_systematic
;
 ? 
;
_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
_audit_creation_date             2017-09-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-09-25 deposited with the CCDC.
2017-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.840(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.354(4)
_cell_length_b                   30.585(3)
_cell_length_c                   18.7881(19)
_cell_measurement_reflns_used    9386
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.76
_cell_measurement_theta_min      2.48
_cell_volume                     18857(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       APEX2(Bruker,2003)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1054
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            175586
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         1.241
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  0.7675
_exptl_absorpt_correction_T_min  0.6531
_exptl_absorpt_correction_type   multi-scan
_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    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7396
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.693
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     943
_refine_ls_number_reflns         17015
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0823P)^2^+68.4620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13013
_reflns_number_total             17015
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03406g2.cif
_cod_data_source_block           3
_cod_original_cell_volume        18858(3)
_cod_database_code               7044368
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.768
_shelx_estimated_absorpt_t_min   0.653
_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
 N1-O1 = N1-O2 = N1-O3
 1.4 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq, Uanis(C19') \\sim Ueq, Uanis(C20) \\sim Ueq, : with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C19(0.6) C19'(0.4) C21(0.5) O4(0.5) O1W(0.5) C21'(0.5)
5.a Ternary CH refined with riding coordinates:
 C5(H5), C12(H12)
5.b Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
5.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39),
  C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C47(H47), C48(H48),
 C49(H49), C50(H50), C51(H51), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57),
  C59(H59), C60(H60), C61(H61), C62(H62), C63(H63), C65(H65), C66(H66),
 C67(H67), C68(H68), C69(H69), C71(H71), C72(H72), C73(H73), C74(H74), C75(H75),
  C77(H77), C78(H78), C79(H79), C80(H80), C81(H81), C83(H83), C84(H84),
 C85(H85), C86(H86), C87(H87), C89(H89), C90(H90), C91(H91), C92(H92), C93(H93)
;
_olex2_submission_special_instructions 'No special instructions were received'