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_4086279
_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'
_chemical_formula_sum            'C34 H40 Co O4 P2 Pd2'
_chemical_formula_weight         846.33
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-18
_audit_creation_method
; 
Olex2 1.2 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) 
;
_cell_angle_alpha                90
_cell_angle_beta                 90.1244(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7355(5)
_cell_length_b                   13.6086(4)
_cell_length_c                   15.8392(5)
_cell_measurement_reflns_used    9402
_cell_measurement_temperature    100
_cell_measurement_theta_max      36.11
_cell_measurement_theta_min      2.36
_cell_volume                     3391.77(18)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_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  0.0412
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            148070
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.252
_diffrn_reflns_theta_min         1.822
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.662
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6799
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2012/1 (Bruker,2012) was used for absorption correction. 
wR2(int) was 0.0663 before and 0.0510 after correction. 
The Ratio of minimum to maximum transmission is 0.9101. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       block
_exptl_crystal_F_000             1700
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.4
_refine_diff_density_max         2.510
_refine_diff_density_min         -1.367
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         16250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0240P)^2^+7.1600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0879
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12956
_reflns_number_total             16250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00579_si_002.cif
_cod_data_source_block           kth19
_cod_database_code               4086279
_shelxl_version_number           2013-3
_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.a Ternary CH refined with riding coordinates: 
 C22(H22), C19(H19), C25(H25), C28(H28) 
2.b Aromatic/amide H refined with riding coordinates: 
 C6(H6), C1(H1), C12(H12), C11(H11), C10(H10), C9(H9), C3(H3), C4(H4), 
 C15(H15), C16(H16), C17(H17), C18(H18) 
2.c Idealised Me refined as rotating group: 
 C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C21(H21A,H21B,H21C), C20(H20A,H20B, 
 H20C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C30(H30A, 
 H30B,H30C) 
;
_shelx_res_checksum              28699
_shelx_hkl_checksum              29276
_olex2_submission_special_instructions 'No special instructions were received'