2-(Methylamido)pyridine-Borane: A Tripod κ(3)-N,H,H Ligand in Trigonal Bipyramidal Rhodium(I) and Iridium(I) Complexes with an Asymmetric Coordination of Its BH3 Group.
Brugos, Javier; Cabeza, Javier A.; García-Álvarez, Pablo; Kennedy, Alan R.; Pérez-Carreño, Enrique; Van der Maelen, Juan F.; Inorganic chemistry 55 (2016) 8905–8912; doi:10.1021/acs.inorgchem.6b01427

data_4348619
_publ_section_title
;
 2-(Methylamido)pyridine-Borane: A Tripod \k(3)-N,H,H Ligand in Trigonal
 Bipyramidal Rhodium(I) and Iridium(I) Complexes with an Asymmetric
 Coordination of Its BH3 Group.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8905
_journal_page_last               8912
_journal_paper_doi               10.1021/acs.inorgchem.6b01427
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C14 H22 B Ir N2'
_chemical_formula_sum            'C14 H22 B Ir N2'
_chemical_formula_weight         421.34
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 120.175(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0435(3)
_cell_length_b                   7.33300(10)
_cell_length_c                   17.5013(5)
_cell_measurement_reflns_used    3460
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      69.2160
_cell_measurement_theta_min      4.2280
_cell_volume                     1336.19(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'X-SEED (Barbour, 1999)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.800
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6091
_diffrn_reflns_point_group_measured_fraction_full 0.800
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        69.326
_diffrn_reflns_theta_max         69.326
_diffrn_reflns_theta_min         4.246
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    19.177
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17186
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    2.094
_exptl_crystal_description       fragment
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.1201
_exptl_crystal_size_mid          0.1140
_exptl_crystal_size_min          0.0687
_refine_diff_density_max         0.542
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0217
_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^)+(0.0269P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0540
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2187
_reflns_number_total             2450
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01427_si_003.cif
_cod_data_source_block           3
_cod_original_cell_volume        1336.18(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4348619
_shelxl_version_number           2014-3
_shelx_res_checksum              60910
_shelx_hkl_checksum              66215