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_1556419
_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 H22 B Cu N P S'
_chemical_formula_sum            'C23 H22 B Cu N P S'
_chemical_formula_weight         449.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 97.6274(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.90994(6)
_cell_length_b                   13.21619(7)
_cell_length_c                   26.83905(13)
_cell_measurement_reflns_used    30315
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.1470
_cell_measurement_theta_min      3.2910
_cell_volume                     4187.20(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.995
_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    0.50    --    5.00   0.00-180.00  356
  2  \w    -84.00  94.00   0.50    0.50    --    5.00  39.00  90.00  356
  3  \w   -179.00  -1.00   0.50    1.00    --  -90.00  57.00-135.57  356
  4  \w   -179.00  -1.00   0.50    1.00    --  -90.00  59.00  53.30  356
  5  \w   -179.00  -1.00   0.50    1.00    --  -90.00  59.00-109.60  356
  6  \w   -179.00  -1.00   0.50    1.00    --  -90.00  10.00-180.00  356
  7  \w   -179.00  -1.00   0.50    1.00    --  -90.00  56.00 164.43  356
  8  \w   -179.00  -1.00   0.50    1.00    --  -90.00  58.00  -0.62  356
  9  \w   -179.00  -1.00   0.50    1.00    --  -90.00  59.00-109.60  356
 10  \w   -109.00 -29.00   0.50    1.00    --  -90.00  57.00  95.13  160
 11  \w    -57.00 -12.00   0.50    1.00    --  -90.00  59.00 131.02   90
 12  \w    -85.00 -28.00   0.50    1.00    --  -90.00  58.00-166.85  114
 13  \w   -178.00-125.00   0.50    1.00    --  -90.00  59.00 -45.63  106
 14  \w   -121.00 -93.00   0.50    1.00    --  -90.00  59.00 -45.63   56
 15  \w   -171.00  -5.00   0.50    1.00    --  -90.00  49.00 120.00  332
 16  \w   -167.00-133.00   0.50    1.00    --  -90.00  59.00  24.77   68
 17  \w   -178.00 -78.00   0.50    1.00    --  -90.00  59.00 179.56  200
 18  \w    -73.00 -39.00   0.50    1.00    --  -90.00  59.00 179.56   68
 19  \w   -178.00-107.00   0.50    1.00    --  -90.00  59.00 131.02  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter \c goniometer'
_diffrn_measurement_device_type
'Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000 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      0.1059522000
_diffrn_orient_matrix_UB_12      -0.0054486000
_diffrn_orient_matrix_UB_13      0.0396273000
_diffrn_orient_matrix_UB_21      -0.0121247000
_diffrn_orient_matrix_UB_22      0.1135270000
_diffrn_orient_matrix_UB_23      0.0112249000
_diffrn_orient_matrix_UB_31      -0.0752005000
_diffrn_orient_matrix_UB_32      -0.0259774000
_diffrn_orient_matrix_UB_33      0.0407039000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0114
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            38239
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.065
_diffrn_reflns_theta_min         3.323
_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    3.175
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.40a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_recrystallization_method
'The material was recrystallised from ether and hexane'
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3963
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.833
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0244
_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^)+(0.0323P)^2^+5.5202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0664
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3908
_reflns_number_total             3963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Inorganics-2019-7-93-1.cif
_cod_data_source_block           1
_cod_database_code               1556419
_chemical_oxdiff_formula         'C20 H22 B N P S Cu'
_chemical_oxdiff_usercomment     JG10
_shelx_estimated_absorpt_t_max   0.806
_shelx_estimated_absorpt_t_min   0.681
_reflns_odcompleteness_completeness 99.42
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     69.95
_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,H,H) groups
2. Shared sites
{C1B, N1A}
{N1B, C1A}
3. Restrained distances
 N1A-B1A
 1.49 with sigma of 0.01
 S1A-C1A \\sim S1B-C1B
 with sigma of 0.02
 N1A-C1A \\sim N1B-C1B
 with sigma of 0.02
 N1A-C5 \\sim N1B-C5
 with sigma of 0.02
 C1A-C2 \\sim C1B-C2
 with sigma of 0.02
 S1A-N1A \\sim S1B-N1B
 with sigma of 0.04
 S1A-C2 \\sim S1B-C2
 with sigma of 0.04
 N1A-C2 \\sim N1B-C2
 with sigma of 0.04
 C1A-C5 \\sim C1B-C5
 with sigma of 0.04
 H1AC-H1AA \\sim H1AC-H1AB \\sim H1AA-H1AB \\sim H1BC-H1BA \\sim H1BC-H1BB
\\sim H1BA-H1BB
 with sigma of 0.04
 B1A-N1A \\sim B1B-N1B
 with sigma of 0.02
 B1A-C1A \\sim B1B-C1B
 with sigma of 0.04
 B1A-C5 \\sim B1B-C5
 with sigma of 0.04
 B1A-H1AC \\sim B1A-H1AA \\sim B1A-H1AB \\sim B1B-H1BC \\sim B1B-H1BA \\sim
B1B-H1BB
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C1B) = Uanis(N1A)
Uanis(N1B) = Uanis(C1A)
5. Rigid body (RIGU) restrains
 S1A, N1A, C1A, B1A, S1B, N1B, C1B, B1B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(H2B)=Sof(H5B)=Sof(S1B)=Sof(N1B)=Sof(C1B)=Sof(B1B)=Sof(H1BA)=Sof(H1BB)=
 Sof(H1BC)=1-FVAR(1)
 Sof(H2A)=Sof(H5A)=Sof(S1A)=Sof(N1A)=Sof(C1A)=Sof(B1A)=Sof(H1AA)=Sof(H1AB)=
 Sof(H1AC)=FVAR(1)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2A), C2(H2B), C3(H3), C4(H4), C5(H5A), C5(H5B), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19),
  C20(H20), C21(H21), C22(H22), C23(H23)
;
_shelx_res_checksum              89145
_shelx_hkl_checksum              48848
_olex2_date_sample_data_collection 2019-02-26
_olex2_date_sample_submission    2019-02-12
_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 JG10
_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 2.964
_oxdiff_exptl_absorpt_empirical_full_min 0.712