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_4086278
_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_absolute_configuration ad
_chemical_formula_moiety         'C36 H44 Fe1 O6 P2 Pd2'
_chemical_formula_sum            'C36 H44 Fe O6 P2 Pd2'
_chemical_formula_weight         903.30
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_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
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0587(5)
_cell_length_b                   14.2422(5)
_cell_length_c                   18.4208(6)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    100
_cell_measurement_theta_max      35.20
_cell_measurement_theta_min      2.64
_cell_volume                     3688.3(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0442
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            80583
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.632
_diffrn_reflns_theta_min         1.807
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.482
_exptl_absorpt_correction_T_max  0.7472
_exptl_absorpt_correction_T_min  0.6227
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2012/1 (Bruker,2012) was used for absorption correction. 
wR2(int) was 0.0665 before and 0.0506 after correction. 
The Ratio of minimum to maximum transmission is 0.8334. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.37
_refine_diff_density_max         1.466
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
; 
 Flack x determined using 5119 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.012(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         16856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+2.4473P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0638
_refine_ls_wR_factor_ref         0.0762
_reflns_Friedel_coverage         0.828
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     0.983
_reflns_number_gt                12733
_reflns_number_total             16856
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00579_si_002.cif
_cod_data_source_block           kth13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_absolute_configuration' value 'AD' changed to 'ad'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_database_code               4086278
_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: 
 C25(H25), C28(H28), C22(H22), C19(H19) 
2.b Aromatic/amide H refined with riding coordinates: 
 C18(H18), C10(H10), C15(H15), C12(H12), C17(H17), C9(H9), C11(H11), C16(H16), 
 C4(H4), C1(H1) 
2.c Idealised Me refined as rotating group: 
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C21(H21A,H21B,H21C), C26(H26A,H26B, 
 H26C), C24(H24A,H24B,H24C), C27(H27A,H27B,H27C), C20(H20A,H20B,H20C), C29(H29A, 
 H29B,H29C), C23(H23A,H23B,H23C), C30(H30A,H30B,H30C) 
;
_shelx_res_checksum              31751
_shelx_hkl_checksum              17697
_olex2_submission_special_instructions 'No special instructions were received'