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_7044371
_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         'C120 H104 Ag4 P4, 10(O)'
_chemical_formula_sum            'C121 H107 Ag4 O9 P4'
_chemical_formula_weight         2260.42
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-09-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-09-26 deposited with the CCDC.
2017-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.531(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.8050(19)
_cell_length_b                   21.229(3)
_cell_length_c                   16.9004(19)
_cell_measurement_reflns_used    9669
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.174
_cell_measurement_theta_min      2.283
_cell_volume                     5907.6(13)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1258
_diffrn_reflns_av_unetI/netI     0.0583
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            119413
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         1.911
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  0.8042
_exptl_absorpt_correction_T_min  0.7026
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2306
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.522
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         10655
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1133P)^2^+17.4564P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1763
_refine_ls_wR_factor_ref         0.2065
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7772
_reflns_number_total             10655
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03406g2.cif
_cod_data_source_block           7
_cod_original_cell_volume        5907.5(12)
_cod_database_code               7044371
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.804
_shelx_estimated_absorpt_t_min   0.703
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C9, C10
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
3. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(O7W)
\\sim Ueq, Uanis(O3W') \\sim Ueq, Uanis(O5W) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(O3W')=1-FVAR(1)
 Sof(O3W)=FVAR(1)
 Fixed Sof: O6W(0.5) O7W(0.5) O4W(0.5) O5W(0.5)
5.a Free rotating group:
 Ag1(Ag2,P1,P2,C1,C2,C3,C4,C5,C6,C7)
5.b Ternary CH refined with riding coordinates:
 C7(H7), C19(H19)
5.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B)
5.d Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51),
 C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59), C60(H60)
;
_olex2_submission_special_instructions 'No special instructions were received'