Bonding and Reactivity of a Dicopper(I) μ-Boryl Cation
Wyss, Chelsea M.; Bitting, Jamie; Bacsa, John; Gray, Thomas G.; Sadighi, Joseph P.; Organometallics 35 (2016) 71–; doi:10.1021/acs.organomet.5b00961

data_4086392
_publ_section_title
;
 Bonding and Reactivity of a Dicopper(I) \m-Boryl Cation
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              71
_journal_paper_doi               10.1021/acs.organomet.5b00961
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'B F4, C60 H80 B Cu2 N4 O2'
_chemical_formula_sum            'C60 H80 B2 Cu2 F4 N4 O2'
_chemical_formula_weight         1113.98
_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   geom
_audit_creation_date             2015-11-09
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2015.10.28 svn.r3245 for OlexSys, GUI svn.r5128)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.979(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2532(16)
_cell_length_b                   22.504(2)
_cell_length_c                   18.5412(19)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.447
_cell_measurement_theta_min      2.450
_cell_volume                     6920.8(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.1-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0916
_diffrn_reflns_av_unetI/netI     0.0877
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44068
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.712
_diffrn_reflns_theta_max         24.712
_diffrn_reflns_theta_min         1.428
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.663
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1070 before and 0.0557 after correction.
The Ratio of minimum to maximum transmission is 0.7937.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_description       prism
_exptl_crystal_F_000             2352
_exptl_crystal_recrystallization_method
;
The material was recrystallised by vapor diffusion. Vapors of 
 3-hexyne were allowed to diffuse into a CH2Cl2 solution of the boryl-bridged dicopper complex.
;
_exptl_crystal_size_max          0.448
_exptl_crystal_size_mid          0.407
_exptl_crystal_size_min          0.152
_refine_diff_density_max         1.144
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     729
_refine_ls_number_reflns         11766
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0719
_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^)+(0.1166P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1833
_refine_ls_wR_factor_ref         0.2174
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6614
_reflns_number_total             11766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00961_si_002.cif
_cod_data_source_block           bb2_sq
_cod_depositor_comments          'Adding full bibliography for 4086392.cif.'
_cod_original_cell_volume        6920.7(12)
_cod_database_code               4086392
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.756
_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. Uiso/Uaniso restraints and constraints
B1B \\sim B1A: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
F1A \\sim F1B: within 1.7A with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(B1A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 N3, C28, N4, C30, C29
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.003
 B1A, F1A, F2A, F3A, F4A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.003
 F4B, F1B, B1B, F2B, F3B
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.003
4. Same fragment restrains
{F1A, F2A, F3A, F4A, B1A} sigma for 1-2: 0.002, 1-3: 0.005
as
{F1B, F2B, F3B, F4B, B1B}
5. Others
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(B1B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(B1A)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C37(H37), C40(H40), C49(H49), C52(H52), C10(H10), C13(H13), C22(H22), C25(H25)
6.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B), C2(H2A,H2B), C3(H3A,H3B)
6.c Aromatic/amide H refined with riding coordinates:
 C33(H33), C34(H34), C35(H35), C45(H45), C46(H46), C47(H47), C6(H6), C7(H7),
 C8(H8), C18(H18), C19(H19), C20(H20), C56(H56), C57(H57), C58(H58), C59(H59)
6.d Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C54(H54A,
 H54B,H54C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              74926
_shelx_hkl_checksum              81993
_shelx_fab_checksum              84214
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id BB2
_olex2_submission_special_instructions 'No special instructions were received'