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_4340820
_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         'C14 H21 B10 Cl N2 O2 Pd, C3 H7 N O'
_chemical_formula_sum            'C17 H28 B10 Cl N3 O3 Pd'
_chemical_formula_weight         572.37
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2013-08-20
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.4690(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0330(5)
_cell_length_b                   20.3495(10)
_cell_length_c                   11.0094(5)
_cell_measurement_reflns_used    9474
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.67
_cell_volume                     2456.0(2)
_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_source
'fine-focus high brilliance microsource sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5014
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.672
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.891
_exptl_absorpt_correction_T_max  0.745554
_exptl_absorpt_correction_T_min  0.621895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1285 before and 0.0463 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1319 before and 0.0655 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       plate
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.104
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+3.3758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4478
_reflns_number_total             5014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5013999_si_002.cif
_cod_data_source_block           ivy314
_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_database_code               4340820
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Sof(H13A)=Sof(H21A)=Sof(O14B)=Sof(H14B)=Sof(O22B)=Sof(H22B)=1-FVAR(1)
 Sof(O14A)=Sof(H14A)=Sof(H13)=Sof(O22A)=Sof(H22A)=Sof(H21)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C13(H13), C13(H13A), C21(H21), C21(H21A)
3.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C24(H24), C19(H19), C26(H26), C18(H18), C16(H16), C25(H25),
 C17(H17), C30(H30)
3.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C32(H32A,H32B,H32C)
3.d Idealised tetrahedral OH refined as rotating group:
 O14A(H14A), O22A(H22A), O14B(H14B), O22B(H22B)
3.e Boron cage BH refined with riding coordinates:
 B7(H7), B3(H3), B9(H9), B8(H8), B10(H10), B12(H12), B4(H4), B5(H5), B6(H6)
;
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.842
_shelxl_version_number           2013-3