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_4340818
_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
'2(C14 H21 B10 Cl N2 O2 Pd), C4 H14 Cl2 N2 Pd, 2(C3 H7 N O)'
_chemical_formula_sum            'C38 H70 B20 Cl4 N8 O6 Pd3'
_chemical_formula_weight         1412.22
_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             2013-06-04
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                99.934(2)
_cell_angle_beta                 101.468(2)
_cell_angle_gamma                102.624(2)
_cell_formula_units_Z            1
_cell_length_a                   10.6774(5)
_cell_length_b                   10.9800(4)
_cell_length_c                   13.2409(6)
_cell_measurement_reflns_used    6143
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.51
_cell_measurement_theta_min      2.80
_cell_volume                     1446.22(11)
_computing_cell_refinement       'Bruker APEX2'
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0228
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21502
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.41
_diffrn_source                   'high brilliance microfocus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.159
_exptl_absorpt_correction_T_max  0.8929
_exptl_absorpt_correction_T_min  0.8735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS, 2012/1'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.997
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+1.9991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0581
_reflns_number_gt                5560
_reflns_number_total             5879
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5013999_si_002.cif
_cod_data_source_block           ivy240g
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' 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               4340818
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2), C13(H13), C21(H21)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C27(H27), C25(H25), C17(H17), C18(H18), C26(H26), C32(H32),
 C24(H24), C19(H19)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C35(H35A,H35B,H35C), C34(H34A,H34B,H34C)
2.d Idealised tetrahedral OH refined as rotating group:
 O22(H22), O14(H14)
2.e Boron cage BH refined with riding coordinates:
 B10(H10), B12(H12), B11(H11), B7(H7), B4(H4), B3(H3), B5(H5), B8(H8), B9(H9)
;