Structure Modulated Electronic Contributions to Metalloenediyne Reactivity: Synthesis and Thermal Bergman Cyclization of MLX2 Compounds
Sibaprasad Bhattacharyya; Aurora E. Clark; Maren Pink; Jeffrey M. Zaleski; Inorganic Chemistry 48 (2009) 3916–3925; doi:10.1021/ic801116q

data_4302037
_publ_section_title
;
Structure Modulated Electronic Contributions to Metalloenediyne Reactivity:
Synthesis and Thermal Bergman Cyclization of MLX2 Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3916
_journal_page_last               3925
_journal_paper_doi               10.1021/ic801116q
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         '(C24 H24 Cl2 N2 Pd), 1.75 (C H2 Cl2)'
_chemical_formula_sum            'C25.75 H27.5 Cl5.5 N2 Pd'
_chemical_formula_weight         666.37
_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                 99.8500(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.9772(7)
_cell_length_b                   14.0789(6)
_cell_length_c                   23.4458(9)
_cell_measurement_reflns_used    9113
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.28
_cell_volume                     5521.4(4)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'XTEL (local library)'
_computing_publication_material  'XCIF (Bruker, 1999), XTEL (local library)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Alatomare et al., 1993)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
'0.30 degree frames measured for 30 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       \w-scans
_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  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            57777
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  978
_diffrn_standards_number         298
_exptl_absorpt_coefficient_mu    1.223
_exptl_absorpt_correction_T_max  0.9414
_exptl_absorpt_correction_T_min  0.7105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing (1995)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2684
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         11327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0321
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+7.1308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                9079
_reflns_number_total             11327
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801116q_si_001.cif
_cod_data_source_block           02035
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'multi-scans' was replaced
with 'multi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C25.75 H27.50 Cl5.50 N2 Pd'
_cod_database_code               4302037