Adding to the Family of Copper Complexes Featuring Borohydride Ligands Based on 2-Mercaptopyridyl Units
Goldsworthy, J.; Thomas, S.D.; Tizzard, G.J.; Coles, S.J.; Owen, G.R.; Inorganics 7 (2019) 93–; doi:10.3390/inorganics7080093

data_1556420
_publ_section_title
;
 Adding to the Family of Copper Complexes Featuring Borohydride Ligands
 Based on 2-Mercaptopyridyl Units
;
_journal_name_full               Inorganics
_journal_page_first              93
_journal_paper_doi               10.3390/inorganics7080093
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'C23 H40 B Cu N P S'
_chemical_formula_sum            'C23 H40 B Cu N P S'
_chemical_formula_weight         467.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                96.9390(10)
_cell_angle_beta                 95.6170(10)
_cell_angle_gamma                112.3730(10)
_cell_formula_units_Z            2
_cell_length_a                   8.16720(10)
_cell_length_b                   9.38370(10)
_cell_length_c                   17.2612(2)
_cell_measurement_reflns_used    26623
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.1570
_cell_measurement_theta_min      2.5930
_cell_volume                     1199.33(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.40a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.40a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.40a (Rigaku OD, 2019)'
_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_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.986
_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    -83.00 -21.00   0.50    0.50    --    5.00  49.00  90.00  124
  2  \w     49.00  92.00   0.50    0.50    --    5.00  49.00  90.00   86
  3  \w    -16.00  45.00   0.50    0.50    --    5.00  49.00  90.00  122
  4  \w     12.00  46.00   0.50    0.50    --  -42.00  53.00 111.68   68
  5  \w    -71.00 -45.00   0.50    0.50    --  -42.00  53.00 111.68   52
  6  \w    -99.00 -73.00   0.50    0.50    --  -52.30  59.00-150.00   52
  7  \w      0.00  34.00   0.50    0.50    --  -52.30  59.00 -30.00   68
  8  \w      6.00  37.00   0.50    0.50    --  -52.30  59.00   0.00   62
  9  \w   -121.00 -96.00   0.50    0.50    --  -52.30  59.00 -90.00   50
 10  \w     10.00  36.00   0.50    0.50    --  -52.30  59.00 120.00   52
 11  \w    -93.00 -54.00   0.50    0.50    --  -52.30  59.00  60.00   78
 12  \w   -140.00-112.00   0.50    0.50    --  -52.30  59.00-150.00   56
 13  \w    -30.00  36.00   0.50    0.50    --  -52.30  59.00 -90.00  132
 14  \w      4.00  32.00   0.50    0.50    --  -52.30  59.00-150.00   56
 15  \w    -88.00 -63.00   0.50    0.50    --  -52.30  59.00 -30.00   50
 16  \w   -137.00-111.00   0.50    0.50    --  -52.30  59.00 -30.00   52
 17  \w   -123.00 -97.00   0.50    0.50    --  -52.30  59.00  60.00   52
 18  \w    -10.00  37.00   0.50    0.50    --  -52.30  59.00  60.00   94
 19  \w    -60.00 -34.00   0.50    0.50    --  -52.30  59.00 -90.00   52
 20  \w   -150.00-125.00   0.50    0.50    --  -66.00  57.00 172.02   50
 21  \w    -12.00  23.00   0.50    0.50    --  -66.00  57.00 172.02   70
 22  \w    -23.00  11.00   0.50    0.50    --  -78.00  56.00 122.68   68
 23  \w   -110.00 -59.00   0.50    0.50    --  -90.00  57.00 -58.75  102
 24  \w   -159.00-114.00   0.50    0.50    --  -90.00  57.00 -58.75   90
 25  \w    -91.00  -1.00   0.50    0.50    --  -90.00  59.00 -20.28  180
 26  \w    -27.00  -1.00   0.50    0.50    --  -90.00  57.00 -13.81   52
 27  \w    -97.00 -44.00   0.50    0.50    --  -90.00  59.00  13.94  106
 28  \w    -39.00  -1.00   0.50    0.50    --  -90.00  59.00  13.94   76
 29  \w   -109.00 -47.00   0.50    0.50    --  -90.00  57.00 -13.81  124
 30  \w   -102.00  -1.00   0.50    0.50    --  -90.00  59.00-103.36  202
 31  \w    -31.00  -2.00   0.50    0.50    --  -90.00  59.00 116.61   58
 32  \w   -119.00 -45.00   0.50    0.50    --  -90.00  59.00 116.61  148
 33  \w   -165.00-122.00   0.50    0.50    --  -90.00  59.00-103.36   86
 34  \w   -156.00-130.00   0.50    0.50    --  -90.00  59.00 -20.28   52
 35  \w   -168.00-134.00   0.50    0.50    --  -90.00  59.00 116.61   68
 36  \w   -116.00  -3.00   0.50    0.50    --  -90.00  58.00-165.39  226
 37  \w    -30.00  -1.00   0.50    0.50    --  -90.00  57.00  59.54   58
 38  \w   -105.00 -71.00   0.50    0.50    --  -90.00  55.00-139.67   68
 39  \w   -175.00  -1.00   0.50    0.50    --  -90.00  58.00-123.71  348
 40  \w    -53.00  -3.00   0.50    0.50    --  -90.00  58.00 126.70  100
 41  \w   -178.00  -1.00   0.50    0.50    --  -90.00  57.00  69.81  354
 42  \w    -60.00  -1.00   0.50    0.50    --  -90.00  55.00-139.67  118
 43  \w    -75.00 -49.00   0.50    0.50    --  -90.00  57.00  59.54   52
 44  \w   -122.00 -60.00   0.50    0.50    --  -90.00  55.00 -89.23  124
 45  \w    -45.00  -1.00   0.50    0.50    --  -90.00  55.00 -89.23   88
 46  \w   -154.00  -2.00   0.50    0.50    --  -90.00  49.00  30.00  304
 47  \w   -109.00 -69.00   0.50    0.50    --  -90.00  58.00 126.70   80
 48  \w    -34.00  -1.00   0.50    0.50    --  -90.00  59.00-175.16   66
 49  \w   -115.00 -40.00   0.50    0.50    --  -90.00  59.00-175.16  150
 50  \w   -116.00 -90.00   0.50    0.50    --  -90.00  59.00 107.23   52
 51  \w    -79.00  -1.00   0.50    0.50    --  -90.00  59.00 107.23  156
 52  \w   -176.00  -1.00   0.50    0.50    --  -90.00  59.00 -42.19  350
 53  \w   -114.00  -1.00   0.50    0.50    --  -90.00  57.00  87.79  226
 54  \w    -28.00  -1.00   0.50    0.50    --  -90.00  58.00 159.07   54
 55  \w   -177.00 -39.00   0.50    0.50    --  -90.00  58.00 159.07  276
 56  \w   -164.00-128.00   0.50    0.50    --  -90.00  59.00-175.16   72
 57  \w    -26.00  -1.00   0.50    0.50    --  -90.00  57.00 -58.75   50
 58  \w   -175.00-124.00   0.50    0.50    --  -90.00  57.00  87.79  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter \c goniometer'
_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      -0.0187269000
_diffrn_orient_matrix_UB_12      0.1570367000
_diffrn_orient_matrix_UB_13      -0.0011538000
_diffrn_orient_matrix_UB_21      -0.0398669000
_diffrn_orient_matrix_UB_22      -0.0360546000
_diffrn_orient_matrix_UB_23      -0.0909594000
_diffrn_orient_matrix_UB_31      -0.2017832000
_diffrn_orient_matrix_UB_32      -0.0807292000
_diffrn_orient_matrix_UB_33      0.0034761000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30937
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.033
_diffrn_reflns_theta_min         2.611
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    2.773
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.40a (Rigaku Oxford Diffraction, 2019)
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    1.296
_exptl_crystal_description       block
_exptl_crystal_F_000             500
_exptl_crystal_recrystallization_method
'The material was recrystallised from ether and hexane'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4471
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0289P)^2^+0.7424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0628
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4402
_reflns_number_total             4471
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Inorganics-2019-7-93-2.cif
_cod_data_source_block           2
_cod_database_code               1556420
_shelx_estimated_absorpt_t_max   0.897
_shelx_estimated_absorpt_t_min   0.635
_reflns_odcompleteness_completeness 98.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_shelx_res_checksum              90327
_shelx_hkl_checksum              19064
_olex2_date_sample_data_collection 2019-02-25
_olex2_date_sample_submission    2019-02-20
_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 JG11
_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 2.133
_oxdiff_exptl_absorpt_empirical_full_min 0.705