Bis{(2-diphenylphosphino)phenyl}mercury: A P-Donor Ligand and Precursor to Mixed Metal-Mercury (d8-d10) Cyclometalated Complexes Containing 2-C6H4PPh2
Martin A. Bennett; Maria Contel; David C. R. Hockless; Lee L. Welling; Anthony C. Willis; Inorganic Chemistry 41 (2002) 844–855; doi:10.1021/ic010890z

data_4317579
_publ_contact_author_address
;
Research School of Chemistry,
Australian National University,
Canberra, A. C. T. 0200, Australia
;
_publ_contact_author_email       ' willis@rsc.anu.edu.au '
_publ_contact_author_fax         ' 61 2 6125 0750 '
_publ_contact_author_name        ' Anthony C. Willis '
_publ_contact_author_phone       ' 61 2 6125 4109 '
_publ_section_title
;
 Bis{(2-diphenylphosphino)phenyl}mercury: A P-Donor Ligand and Precursor
 to Mixed Metal-Mercury (d8-d10) Cyclometalated Complexes Containing
 2-C6H4PPh2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              844
_journal_page_last               855
_journal_paper_doi               10.1021/ic010890z
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C72 H56  Hg2 O P4 Pd , C7 H8, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C79.5 H65 Cl Hg2 O P4 Pd'
_chemical_formula_weight         1703.32
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2001-07-27
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
1999-04-17 - Report on C79.50 H65 Cl Hg2 O P4 Pd
             by David C. R. Hockless
             for Martin A. Bennett
2001-07-27 - Anthony C. Willis  produces cif
             acw becomes e-mail contact
2000-07-27 - passes checkcif with some warnings
;
_cell_angle_alpha                93.830(7)
_cell_angle_beta                 93.664(6)
_cell_angle_gamma                104.378(7)
_cell_formula_units_Z            2
_cell_length_a                   13.199(1)
_cell_length_b                   15.273(2)
_cell_length_c                   17.850(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193.2
_cell_measurement_theta_max      50.0
_cell_measurement_theta_min      49.2
_cell_volume                     3465.8(6)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
SIR92 (Altomare, et. al. 1994)
;
_diffrn_ambient_temperature      193.2
_diffrn_measurement_device_details
;
Rigaku AFC6R diffractometer with extended arm and
evacuated collimator and beam tunnel.
Data cannot be collected beyond \y 60 deg in this configuration.
;
_diffrn_measurement_device_type  'Rigaku AFC6R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.07234
_diffrn_orient_matrix_UB_12      -0.01017
_diffrn_orient_matrix_UB_13      0.01718
_diffrn_orient_matrix_UB_21      -0.03039
_diffrn_orient_matrix_UB_22      -0.01663
_diffrn_orient_matrix_UB_23      -0.05333
_diffrn_orient_matrix_UB_31      -0.00168
_diffrn_orient_matrix_UB_32      -0.06498
_diffrn_orient_matrix_UB_33      0.00593
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.03186
_diffrn_reflns_av_sigmaI/netI    0.050
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10765
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         60.07
_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        2.25
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    10.945
_exptl_absorpt_correction_T_max  .174
_exptl_absorpt_correction_T_min  .121
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_meas      ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1666.00
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.19
_refine_diff_density_min         -0.99
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.784
_refine_ls_goodness_of_fit_ref   1.890
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     808
_refine_ls_number_reflns         8645
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.1470
_refine_ls_shift/su_mean         0.0350
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0339
_refine_ls_wR_factor_ref         0.0326
_reflns_number_gt                8645
_reflns_number_total             10314
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            ic010890z_6.cif
_cod_data_source_block           CON17
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3465.8(5)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C79.50 H65 Cl Hg2 O P4 Pd '
_cod_database_code               4317579