Supramolecular Structures from Polycarbene Ligands and Transition Metal Ions
Rit, Arnab; Pape, Tania; Hepp, Alexander; Hahn, F. Ekkehardt; Organometallics 30 (2011) 334–347; doi:10.1021/om101102j

data_4063416
_publ_section_title
;
 Supramolecular Structures from Polycarbene Ligands and Transition Metal
 Ions
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              334
_journal_page_last               347
_journal_paper_doi               10.1021/om101102j
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C44 H52.5 Ag3 F18 N12 O0.75 P3'
_chemical_formula_weight         1520.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.2160(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.493(2)
_cell_length_b                   19.0350(13)
_cell_length_c                   21.5033(15)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1
_cell_volume                     13894.7(16)
_computing_cell_refinement       'APEX2(Bruker AXS, 2007)'
_computing_data_collection       'APEX2(Bruker AXS, 2007)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2007 )'
_computing_molecular_graphics
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement
;
SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_structure_solution
;
SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0693
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            81217
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.992
_exptl_absorpt_correction_T_max  0.9160
_exptl_absorpt_correction_T_min  0.8187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports ratio of Tmin/Tmax = 0.720994   

;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent sticks'
_exptl_crystal_F_000             6036
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         3.659
_refine_diff_density_min         -1.504
_refine_diff_density_rms         0.217
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1410
_refine_ls_number_reflns         39289
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1352P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1812
_refine_ls_wR_factor_ref         0.2089
_reflns_number_gt                28304
_reflns_number_total             39289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101102j_si_005.cif
_cod_data_source_block           sad
_cod_original_cell_volume        13894.8(17)
_cod_original_sg_symbol_H-M      C2
_cod_original_formula_sum        'C44 H52.50 Ag3 F18 N12 O0.75 P3'
_cod_database_code               4063416