Synthesis and Characterization of the Homologous M-M Bonded Series Ar'MMAr' (M = Zn, Cd, or Hg; Ar' = C6H3-2,6-(C6H3-2,6-Pri2)2) and Related Arylmetal Halides and Hydride Species
Zhongliang Zhu; Marcin Brynda; Robert J. Wright; Roland C. Fischer; W. Alexander Merrill; Eric Rivard; Robert Wolf; James C. Fettinger; Marilyn M. Olmstead; Philip P. Power; Journal of the American Chemical Society 129 (2007) 10847–10857; doi:10.1021/ja072682x

data_4109855
_publ_contact_author_address
;
Department of Chemistry
University of California
Davis
CA 95616
UNITED STATES OF AMERICA
;
_publ_contact_author_email       PPPOWER@UCDAVIS.EDU
_publ_contact_author_name        'P. P. Power'
_publ_section_title
;
 Synthesis and Characterization of the Homologous M-M Bonded Series
 Ar'MMAr' (M = Zn, Cd, or Hg; Ar' = C6H3-2,6-(C6H3-2,6-Pri2)2) and Related
 Arylmetal Halides and Hydride Species
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10847
_journal_page_last               10857
_journal_paper_doi               10.1021/ja072682x
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C60 H74 I2 Zn2, 2(C7 H8)'
_chemical_formula_sum            'C74 H90 I2 Zn2'
_chemical_formula_weight         1364.04
_chemical_melting_point_gt       633
_chemical_name_common            'Compound 1'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 121.322(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9561(4)
_cell_length_b                   22.5253(6)
_cell_length_c                   24.9183(6)
_cell_measurement_reflns_used    8065
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      29.82
_cell_measurement_theta_min      2.32
_cell_volume                     6691.8(4)
_computing_cell_refinement       'SAINT (7.06a) (Bruker, 2004)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT (7.06a) (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            68042
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.32
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    1.679
_exptl_absorpt_correction_T_max  0.6789
_exptl_absorpt_correction_T_min  0.6114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       block
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         13168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0776P)^2^+6.6781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0841
_reflns_number_gt                9819
_reflns_number_total             13168
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja072682xsi20070417_053248_1.cif
_cod_data_source_block           rjw83
_cod_original_cell_volume        6691.8(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4109855