Heterometallic Effects in Trinuclear Complexes Supported byp-Terphenyl Diphosphine Ligands
Horak, Kyle T.; Lin, Sibo; Rittle, Jonathan; Agapie, Theodor; Organometallics 34 (2015) 4429–; doi:10.1021/acs.organomet.5b00579

data_4086277
_publ_section_title
;
 Heterometallic Effects in Trinuclear Complexes Supported byp-Terphenyl
 Diphosphine Ligands
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4429
_journal_paper_doi               10.1021/acs.organomet.5b00579
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety
'C34 H40 Co O4 P2 Pd2, B F4, 0.5(C6 H6), 1.5(C2 H3 N)'
_chemical_formula_sum            'C40 H47.5 B Co F4 N1.5 O4 P2 Pd2'
_chemical_formula_weight         1033.77
_chemical_name_systematic
;
 ?
;
_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
_audit_creation_date             2015-03-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.490(3)
_cell_angle_beta                 114.618(2)
_cell_angle_gamma                105.162(2)
_cell_formula_units_Z            4
_cell_length_a                   15.9326(8)
_cell_length_b                   16.5136(9)
_cell_length_c                   18.4384(10)
_cell_measurement_reflns_used    9839
_cell_measurement_temperature    100
_cell_measurement_theta_max      48.05
_cell_measurement_theta_min      2.25
_cell_volume                     4218.4(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            179151
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.289
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.367
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0588 before and 0.0494 after correction.
The Ratio of minimum to maximum transmission is 0.8869.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_description       block
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1019
_refine_ls_number_reflns         17247
_refine_ls_number_restraints     363
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0264
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+7.3884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0772
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14742
_reflns_number_total             17247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00579_si_002.cif
_cod_data_source_block           kth12_0m
_cod_original_formula_sum        'C40 H47.50 B Co F4 N1.50 O4 P2 Pd2'
_cod_database_code               4086277
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.842
_shelx_estimated_absorpt_t_min   0.604
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Ternary CH refined with riding coordinates:
 C19(H19), C22(H22), C25(H25), C28(H28), C19A(H19A), C22A(H22A), C25A(H25A),
 C28A(H28A)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C1A(H1A), C3A(H3A), C4A(H4A), C6A(H6A),
  C9A(H9A), C10A(H10A), C11A(H11A), C12A(H12A), C15A(H15A), C16A(H16A),
 C17A(H17A), C18A(H18A), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43),
 C44(H44)
3.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C20A(H20D,H20E,H20F), C21A(H21D,H21E,H21F), C23A(H23D,H23E,H23F),
 C24A(H24D,H24E,H24F), C26A(H26D,H26E,H26F), C27A(H27D,H27E,H27F), C29A(H29D,
 H29E,H29F), C30A(H30D,H30E,H30F), C38(H38A,H38B,H38C), C36(H36A,H36B,H36C),
 C36A(H36D,H36E,H36F)
;
_shelx_res_checksum              16013
_shelx_hkl_checksum              54567
_olex2_submission_special_instructions 'No special instructions were received'