Unexpected Formation of Early Late Heterobimetallic Complexes from Transition Metal Frustrated Lewis Pairs.
Chapman, Andy M.; Flynn, Stephanie R.; Wass, Duncan F.; Inorganic chemistry 55 (2016) 1017–1021; doi:10.1021/acs.inorgchem.5b01424

data_4344710
_publ_section_title
;
 Unexpected Formation of Early Late Heterobimetallic Complexes from
 Transition Metal Frustrated Lewis Pairs.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1017
_journal_page_last               1021
_journal_paper_doi               10.1021/acs.inorgchem.5b01424
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C23 H33 F6 O P Pt Zr'
_chemical_formula_sum            'C23 H33 F6 O P Pt Zr'
_chemical_formula_weight         756.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_date             2015-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                78.199(4)
_cell_angle_beta                 88.772(5)
_cell_angle_gamma                71.330(4)
_cell_formula_units_Z            2
_cell_length_a                   8.4592(8)
_cell_length_b                   9.9099(10)
_cell_length_c                   16.1139(17)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.71
_cell_measurement_theta_min      2.22
_cell_volume                     1251.3(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'Bruker area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_device_type  'Bruker Apex II kappa CCDC area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21217
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.731
_diffrn_reflns_theta_min         2.323
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.123
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5045
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0879 before and 0.0326 after correction.
The Ratio of minimum to maximum transmission is 0.6766.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.009
_exptl_crystal_description       block
_exptl_crystal_F_000             732
_exptl_crystal_recrystallization_method
'Layered benzene:hexane - slow evaporation at room temperature'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.376
_refine_diff_density_min         -2.087
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.381
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5826
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.377
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+8.9936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5774
_reflns_number_total             5826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01424_si_002.cif
_cod_data_source_block           amc352
_cod_database_code               4344710
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed Sof: C16(0.5398) H16A(0.5398) H16B(0.5398) H16C(0.5398) C17(0.5398)
 H17A(0.5398) H17B(0.5398) H17C(0.5398) C18(0.5398) H18A(0.5398) H18B(0.5398)
 H18C(0.5398) C16A(0.4602) H16D(0.4602) H16E(0.4602) H16F(0.4602) C17A(0.4602)
 H17D(0.4602) H17E(0.4602) H17F(0.4602) C18A(0.4602) H18D(0.4602) H18E(0.4602)
 H18F(0.4602)
 Fixed Uiso: H1(0.033) H2(0.04) H3(0.051) H4(0.06) H5(0.05) H6(0.029)
 H7(0.035) H8(0.041) H9(0.045) H10(0.04) H12A(0.021) H12B(0.021) H20A(0.095)
 H20B(0.095) H20C(0.095) H21A(0.079) H21B(0.079) H21C(0.079) H22A(0.086)
 H22B(0.086) H22C(0.086) H23A(0.062) H23B(0.062) H23C(0.062) H16A(0.034)
 H16B(0.034) H16C(0.034) H17A(0.057) H17B(0.057) H17C(0.057) H18A(0.062)
 H18B(0.062) H18C(0.062) H16D(0.055) H16E(0.055) H16F(0.055) H17D(0.063)
 H17E(0.063) H17F(0.063) H18D(0.026) H18E(0.026) H18F(0.026)
 Fixed X: H1(-0.1348) H2(-0.1662) H3(-0.0404) H4(0.0647) H5(0.0051) H6(0.5438)
 H7(0.3437) H8(0.247) H9(0.3825) H10(0.5683) H12A(0.1145) H12B(0.299)
 H20A(0.231) H20B(0.1101) H20C(0.2996) H21A(0.2492) H21B(0.0641) H21C(0.0921)
 H22A(-0.0641) H22B(-0.1018) H22C(-0.0227) H23A(0.2828) H23B(0.4674)
 H23C(0.3151) H16A(0.5808) H16B(0.6023) H16C(0.7335) H17A(0.6897) H17B(0.5299)
 H17C(0.5203) H18A(0.4532) H18B(0.5133) H18C(0.647) H16D(0.5615) H16E(0.5884)
 H16F(0.7232) H17D(0.7225) H17E(0.5975) H17F(0.5566) H18D(0.6363) H18E(0.467)
 H18F(0.46)
 Fixed Y: H1(1.0421) H2(1.0241) H3(1.1939) H4(1.3244) H5(1.2351) H6(0.7672)
 H7(0.8566) H8(1.1294) H9(1.2096) H10(0.9834) H12A(0.5903) H12B(0.5131)
 H20A(0.8757) H20B(0.8234) H20C(0.7222) H21A(0.5098) H21B(0.5903) H21C(0.5294)
 H22A(0.7624) H22B(0.8242) H22C(0.9061) H23A(1.1911) H23B(1.1216) H23C(1.1992)
 H16A(0.575) H16B(0.7142) H16C(0.556) H17A(0.6042) H17B(0.7482) H17C(0.6057)
 H18A(0.4133) H18B(0.3891) H18C(0.3757) H16D(0.4938) H16E(0.6495) H16F(0.5101)
 H17D(0.5995) H17E(0.7567) H17F(0.6719) H18D(0.3815) H18E(0.4565) H18F(0.3939)
 Fixed Z: H1(0.2117) H2(0.3691) H3(0.416) H4(0.2869) H5(0.1604) H6(0.386)
 H7(0.4957) H8(0.4609) H9(0.3257) H10(0.2816) H12A(0.2486) H12B(0.2887)
 H20A(0.0151) H20B(-0.0366) H20C(-0.013) H21A(0.0693) H21B(0.0279) H21C(0.1282)
 H22A(0.1573) H22B(0.0574) H22C(0.1124) H23A(0.0729) H23B(0.1162) H23C(0.169)
 H16A(0.2946) H16B(0.2311) H16C(0.2328) H17A(0.0836) H17B(0.0694) H17C(0.0405)
 H18A(0.1445) H18B(0.2415) H18C(0.1693) H16D(0.2978) H16E(0.2735) H16F(0.2489)
 H17D(0.1077) H17E(0.1142) H17F(0.0472) H18D(0.1535) H18E(0.0958) H18F(0.1951)
;
_shelx_res_checksum              24620
_shelx_hkl_checksum              65882
_olex2_submission_original_sample_id amc352
_olex2_submission_special_instructions 'No special instructions were received'