Synthesis and characterization of the first metallacyclooctane
Sivaramakrishna, Akella; Su, Hong; Moss, John R.; Dalton Transactions  (2008) 2228–2231; doi:10.1039/b800843b

data_7003871
_publ_section_title
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 Synthesis and characterization of the first metallacyclooctane
;
_journal_issue                   17
_journal_name_full               'Dalton Transactions'
_journal_page_first              2228
_journal_page_last               2231
_journal_paper_doi               10.1039/b800843b
_journal_year                    2008
_chemical_formula_moiety         C37H44P2Pt
_chemical_formula_sum            'C37 H44 P2 Pt'
_chemical_formula_weight         745.75
_chemical_melting_point          394.1(10)
_chemical_name_systematic
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Bis(diphenylphosphino)propane-bis(1-pentenyl)platinum(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.3020(10)
_cell_angle_beta                 75.6290(10)
_cell_angle_gamma                89.3610(10)
_cell_formula_units_Z            4
_cell_length_a                   13.36530(10)
_cell_length_b                   13.99500(10)
_cell_length_c                   18.35420(10)
_cell_measurement_reflns_used    80402
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      1.15
_cell_volume                     3324.19(4)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT program (Nonius, 2000)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius Kappa CCD diffractometer'
_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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            80402
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    4.341
_exptl_absorpt_correction_T_max  0.5621
_exptl_absorpt_correction_T_min  0.5088
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.212
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       0.00083(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         13036
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0166P)^2^+4.1248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0586
_reflns_number_gt                10902
_reflns_number_total             13036
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b800843b.txt
_cod_data_source_block           rk18
_cod_depositor_comments
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The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '120-122\%C' was changed to
'394.1(10)' - it was converted from degrees Celsius(C) to Kelvins(K),
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7003871