Synthesis, Structure, and Catalytic Applications for ortho- and meta-Carboranyl Based NBN Pincer-Pd Complexes.
Tsang, Min Ying; Viñas, Clara; Teixidor, Francesc; Planas, José Giner; Conde, Nerea; SanMartin, Raul; Herrero, María Teresa; Domínguez, Esther; Lledós, Agustí; Vidossich, Pietro; Choquesillo-Lazarte, Duane; Inorganic chemistry 53 (2014) 9284–9295; doi:10.1021/ic5013999

data_4340819
_publ_section_title
;
 Synthesis, Structure, and Catalytic Applications for ortho- and
 meta-Carboranyl Based NBN Pincer-Pd Complexes.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9284
_journal_page_last               9295
_journal_paper_doi               10.1021/ic5013999
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C16 H25 B10 Cl N2 O2 Pd'
_chemical_formula_sum            'C16 H25 B10 Cl N2 O2 Pd'
_chemical_formula_weight         527.33
_chemical_name_systematic
;
 ? 
;
_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_date             2013-09-25
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                68.9240(10)
_cell_angle_beta                 67.4490(10)
_cell_angle_gamma                67.4990(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9166(4)
_cell_length_b                   10.7176(4)
_cell_length_c                   12.7142(5)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.22
_cell_measurement_theta_min      2.41
_cell_volume                     1116.52(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15319
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.32
_diffrn_source                   'high brilliance microfocus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.969
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1261 before and 0.0413 after correction.
The Ratio of minimum to maximum transmission is 0.8554.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         4576
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+1.2727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0649
_reflns_number_gt                4408
_reflns_number_total             4576
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5013999_si_002.cif
_cod_data_source_block           ivy302
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/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 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4340818--4340820.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4340819
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C22A) = Uanis(C22B)
Uanis(C13A) = Uanis(C13B)
3. Others
 Sof(O23B)=Sof(H23B)=Sof(C22B)=Sof(H22B)=Sof(O14B)=Sof(H14B)=Sof(C13B)=
 Sof(H13B)=1-FVAR(1)
 Sof(C13A)=Sof(H13A)=Sof(O23A)=Sof(H23A)=Sof(O14A)=Sof(H14A)=Sof(C22A)=
 Sof(H22A)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C13A(H13A), C22A(H22A), C22B(H22B), C13B(H13B)
4.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C27(H27), C26(H26), C16(H16), C18(H18), C17(H17)
4.c Tetrahedral OH refined with riding coordinates:
 O23B(H23B)
4.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C29(H29A,H29B,H29C)
4.e Idealised tetrahedral OH refined as rotating group:
 O23A(H23A), O14A(H14A), O14B(H14B)
4.f Boron cage BH refined with riding coordinates:
 B6(H6), B11(H11), B8(H8), B10(H10), B7(H7), B4(H4), B5(H5), B9(H9), B12(H12)
;