Metal-ligand cooperative κ<sup>1</sup>-<i>N</i>-pyrazolate Cp*Rh<sup>III</sup>-catalysts for dehydrogenation of dimethylamine-borane at room temperature.
Pal, Shrinwantu; Iwasaki, Takanori; Nozaki, Kyoko; Dalton transactions (Cambridge, England : 2003) 50 (2021) 7938–7943; doi:10.1039/d1dt01705e

data_7707565
_publ_section_title
;
 Metal-ligand cooperative \k<sup>1</sup>-<i>N</i>-pyrazolate
 Cp*Rh<sup>III</sup>-catalysts for dehydrogenation of dimethylamine-borane
 at room temperature.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7938
_journal_page_last               7943
_journal_paper_doi               10.1039/d1dt01705e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C20 H30 Cl N4 Rh'
_chemical_formula_sum            'C20 H30 Cl N4 Rh'
_chemical_formula_weight         464.84
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-03-15 deposited with the CCDC.	2021-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.79000(10)
_cell_length_b                   13.1300(2)
_cell_length_c                   17.9482(2)
_cell_measurement_reflns_used    31759
_cell_measurement_temperature    93.15
_cell_measurement_theta_max      28.3800
_cell_measurement_theta_min      2.2760
_cell_volume                     2071.45(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.72a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.72a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.72a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.952
_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    -84.00  94.00   0.50    1.00    --    5.00  43.00 -79.00  356
  2  \w   -105.00  74.00   0.50    1.00    --  -15.80  43.00 -79.00  358
  3  \w    -84.00  94.00   0.50    1.00    --    5.00   9.00  30.00  356
  4  \w   -105.00  74.00   0.50    1.00    --  -15.80  18.00  30.00  358
  5  \w   -105.00  59.00   0.50    1.00    --  -15.80  55.00-180.00  328
  6  \w   -105.00 -34.00   0.50    1.00    --  -15.80  18.00-120.00  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0544956000
_diffrn_orient_matrix_UB_12      0.0117512000
_diffrn_orient_matrix_UB_13      0.0278460000
_diffrn_orient_matrix_UB_21      0.0096316000
_diffrn_orient_matrix_UB_22      -0.0526969000
_diffrn_orient_matrix_UB_23      0.0073643000
_diffrn_orient_matrix_UB_31      0.0586972000
_diffrn_orient_matrix_UB_32      -0.0022619000
_diffrn_orient_matrix_UB_33      -0.0270561000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34744
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.306
_diffrn_reflns_theta_min         2.269
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Mo) X-ray DW Source'
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.72a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       irregular
_exptl_crystal_F_000             960
_exptl_crystal_recrystallization_method
'crystalized from a THF solution by vapour diffusion with hexane at room temperature'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.45(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         4782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0185
_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^)+(0.0316P)^2^+0.6307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0493
_reflns_Friedel_coverage         0.766
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.952
_reflns_number_gt                4746
_reflns_number_total             4782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01705e3.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7707565--7707566.cif.'
_cod_database_code               7707565
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C80 H116 Cl4 N16 Rh4 '
_chemical_oxdiff_usercomment
'0.50 0.40 0.30 orange chunk THF hexane parafin oil -180deg'
_shelx_estimated_absorpt_t_max   0.761
_shelx_estimated_absorpt_t_min   0.644
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.55(3)
 0.45(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7)
3.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C9(H9A,H9B,H9C), C5(H5A,H5B,H5C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C10(H10A,H10B,H10C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              75248
_shelx_hkl_checksum              19353
_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 1.525
_oxdiff_exptl_absorpt_empirical_full_min 0.758