Intermetallic Bonds in Metallophilic Mercuraazametallamacrocycles of Synthetic Design
Patel, Upali; Sharma, Sagar; Singh, Harkesh B.; Dey, Sandip; Jain, Vimal K.; Wolmershäuser, Gotthelf; Butcher, Ray J.; Organometallics 29 (2010) 4265–; doi:10.1021/om100297v

data_4066105
_publ_section_title
;
 Intermetallic Bonds in Metallophilic Mercuraazametallamacrocycles of
 Synthetic Design
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              4265
_journal_paper_doi               10.1021/om100297v
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         '2(C40 H28 Cl2 Hg2 N4 Pd), C3 H6 O'
_chemical_formula_sum            'C41.5 H31 Cl2 Hg2 N4 O0.5 Pd'
_chemical_formula_weight         1172.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.957(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            32
_cell_length_a                   41.2863(7)
_cell_length_b                   19.3267(2)
_cell_length_c                   41.0150(7)
_cell_measurement_reflns_used    19342
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      73.4914
_cell_measurement_theta_min      4.0950
_cell_volume                     30761.7(9)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.5081
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            67399
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         73.78
_diffrn_reflns_theta_min         4.10
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    19.336
_exptl_absorpt_correction_T_max  0.469
_exptl_absorpt_correction_T_min  0.041
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.025
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'long plate'
_exptl_crystal_F_000             17664
_exptl_crystal_size_max          0.4846
_exptl_crystal_size_mid          0.1304
_exptl_crystal_size_min          0.0555
_refine_diff_density_max         4.570
_refine_diff_density_min         -1.275
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1841
_refine_ls_number_reflns         29988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0799P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1416
_reflns_number_gt                15678
_reflns_number_total             29988
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om100297v_si_002.cif
_cod_data_source_block           9a
_cod_original_cell_volume        30761.7(8)
_cod_database_code               4066105