Preparation and Reactivity of Rhodium and Iridium Complexes Containing a Methylborohydride Based Unit Supported by Two 7-Azaindolyl Heterocycles
Da Costa, Rosenildo Correa; Rawe, Benjamin W.; Tsoureas, Nikolaos; Haddow, Mairi F.; Sparkes, Hazel Anne; Tizzard, Graham J.; Coles, Simon; Owen, Gareth Richard; Dalton Transactions  (2018) –; doi:10.1039/C8DT02311E

data_7047064
_publ_section_title
;
 Preparation and Reactivity of Rhodium and Iridium Complexes Containing a
 Methylborohydride Based Unit Supported by Two 7-Azaindolyl Heterocycles
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT02311E
_journal_year                    2018
_chemical_formula_moiety         'C23 H26 B N4 Rh'
_chemical_formula_sum            'C23 H26 B N4 Rh'
_chemical_formula_weight         472.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-04
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-06-04 deposited with the CCDC.
2018-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.767(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.5731(3)
_cell_length_b                   16.5975(4)
_cell_length_c                   17.2681(3)
_cell_measurement_reflns_used    10562
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.0800
_cell_measurement_theta_min      3.1190
_cell_volume                     4038.80(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -34.00  80.00   1.00    3.00    --   -9.70  38.00 120.00  114
  2  \w    -99.00  20.00   1.00    3.00    --   -9.70 -57.00-180.00  119
  3  \w    -43.00  80.00   1.00    3.00    --   -9.70  72.00   0.00  123
  4  \w    -38.00 -13.00   1.00    3.00    --   -9.70  54.00-118.00   25
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0295391000
_diffrn_orient_matrix_UB_12      0.0272191000
_diffrn_orient_matrix_UB_13      -0.0268853000
_diffrn_orient_matrix_UB_21      -0.0358411000
_diffrn_orient_matrix_UB_22      -0.0048192000
_diffrn_orient_matrix_UB_23      0.0207536000
_diffrn_orient_matrix_UB_31      0.0194118000
_diffrn_orient_matrix_UB_32      0.0325901000
_diffrn_orient_matrix_UB_33      0.0255146000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46283
_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         27.483
_diffrn_reflns_theta_min         2.440
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_recrystallization_method
'The material was recrystallised from hexane by slow evaporation'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.043
_refine_diff_density_min         -1.404
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         9257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0571
_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^)+(0.0822P)^2^+1.5150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1559
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6997
_reflns_number_total             9257
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02311e2.cif
_cod_data_source_block           2a
_cod_database_code               7047064
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C23 H26 B N4 Rh'
_chemical_oxdiff_usercomment     NC19
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.919
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All B(H) groups, All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C20(H20), C115(H115), C116(H116), C117(H117),
 C120(H120)
2.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B), C22(H22A,H22B), C118(H11D,
 H11E), C119(H11F,H11G), C121(H12A,H12B), C122(H12C,H12D)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C102(H102), C103(H103), C104(H104), C105(H105), C106(H106),
 C108(H108), C109(H109), C110(H110), C111(H111), C112(H112)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C114(H11A,H11B,H11C)
;
_shelx_res_checksum              65815
_olex2_date_sample_data_collection 2018-02-09
_olex2_date_sample_submission    2018-01-12
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id NC19
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.272
_oxdiff_exptl_absorpt_empirical_full_min 0.695