A neutral, acyclic, borataalkene-like ligand for group 11 metals: L- and Z-type ligands side by side.
Krämer, Felix; Radius, Michael; Berberich, Helga; Fernández, Israel; Breher, Frank; Chemical communications (Cambridge, England) 58 (2022) 3905–3908; doi:10.1039/d2cc00199c

data_7129741
_publ_section_title
;
 A neutral, acyclic, borataalkene-like ligand for group 11 metals: L- and
 Z-type ligands side by side.
;
_journal_issue                   24
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3905
_journal_page_last               3908
_journal_paper_doi               10.1039/d2cc00199c
_journal_volume                  58
_journal_year                    2022
_chemical_formula_moiety         'C24 H28 Au B Cl P'
_chemical_formula_sum            'C24 H28 Au B Cl P'
_chemical_formula_weight         590.66
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-02-07 deposited with the CCDC.	2022-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.133(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.1732(10)
_cell_length_b                   13.6458(6)
_cell_length_c                   19.7945(11)
_cell_measurement_reflns_used    36687
_cell_measurement_temperature    200
_cell_measurement_theta_max      29.45
_cell_measurement_theta_min      1.43
_cell_volume                     4620.1(4)
_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      200
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41914
_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         27.000
_diffrn_reflns_theta_min         1.815
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    6.58
_exptl_absorpt_correction_T_max  0.4577
_exptl_absorpt_correction_T_min  0.1221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2304
_exptl_crystal_recrystallization_method
'The material was recrystallised from DCM by slow evaporation'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.383
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.469
_refine_diff_density_min         -1.793
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       0.00067(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         10070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0528
_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^)+(0.1042P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1548
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7634
_reflns_number_total             10070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc00199c2.cif
_cod_data_source_block           mr606
_cod_depositor_comments          'Adding full bibliography for 7129741.cif.'
_cod_database_code               7129741
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.291
_shelx_estimated_absorpt_t_min   0.111
_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 C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C43(H43A,H43B), C91(H91A,H91B), C93(H93A,H93B)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36),
  C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C72(H72), C73(H73),
 C74(H74), C75(H75), C76(H76), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C52(H52A,H52B,
 H52C), C92(H92A,H92B,H92C), C94(H94A,H94B,H94C)
;
_shelx_res_checksum              37297
_shelx_hkl_checksum              15700
_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 MR606
_olex2_submission_special_instructions 'No special instructions were received'