Robust dicopper(i) μ-boryl complexes supported by a dinucleating naphthyridine-based ligand.
Ríos, Pablo; See, Matthew S.; Handford, Rex C.; Teat, Simon J.; Tilley, T. Don; Chemical science 13 (2022) 6619–6625; doi:10.1039/d2sc00848c

data_1566968
_publ_section_title
;
 Robust dicopper(i) \m-boryl complexes supported by a dinucleating
 naphthyridine-based ligand.
;
_journal_issue                   22
_journal_name_full               'Chemical science'
_journal_page_first              6619
_journal_page_last               6625
_journal_paper_doi               10.1039/d2sc00848c
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C34 H29 Cu2 F2 N6 O, C6 H4 F2, C2 F6 N O4 S2'
_chemical_formula_sum            'C42 H33 Cu2 F10 N7 O5 S2'
_chemical_formula_weight         1096.95
_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   geom
_audit_creation_date             2021-12-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-12-23 deposited with the CCDC.	2022-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                63.797(3)
_cell_angle_beta                 69.859(2)
_cell_angle_gamma                65.255(3)
_cell_formula_units_Z            2
_cell_length_a                   12.9678(3)
_cell_length_b                   14.3694(4)
_cell_length_c                   14.5813(4)
_cell_measurement_reflns_used    33032
_cell_measurement_temperature    100
_cell_measurement_theta_max      78.3720
_cell_measurement_theta_min      3.6030
_cell_volume                     2171.18(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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    108.00 175.00   0.50    0.50    --  107.75  30.00   0.00  134
  2  \w     81.00 124.00   0.50    0.50    --   50.71  77.00-180.00   86
  3  \w     92.00 169.00   0.50    0.50    --  107.75  77.00-180.00  154
  4  \w     94.00 170.00   0.50    0.50    --  107.75  45.00  60.00  152
  5  \w    114.00 174.00   0.50    0.50    --  107.75  15.00 120.00  120
  6  \w     32.00 108.00   0.50    0.50    --  107.75-111.00  90.00  152
  7  \w     40.00  85.00   0.50    0.50    --  107.75-111.00 150.00   90
  8  \w     52.00  78.00   0.50    0.50    --  107.75-111.00  60.00   52
  9  \w     32.00  65.00   0.50    0.50    --  107.75 -94.00   0.00   66
 10  \w     33.00  61.00   0.50    0.50    --  107.75-111.00 -60.00   56
 11  \w     64.00  97.00   0.50    0.50    --  107.75-111.00 -60.00   66
 12  \w     62.00 109.00   0.50    0.50    --  107.75-111.00 -90.00   94
 13  \w     48.00  99.00   0.50    0.50    --  107.75 -94.00-180.00  102
 14  \w     31.00 109.00   0.50    0.50    --  107.75-111.00-120.00  156
 15  \w     38.00 103.00   0.50    0.50    --  107.75 -94.00 -60.00  130
 16  \w     73.00 105.00   0.50    0.50    --  107.75 -94.00 -30.00   64
 17  \w     40.00  67.00   0.50    0.50    --  107.75 -94.00 -30.00   54
 18  \w     74.00 100.00   0.50    0.50    --  107.75 -94.00   0.00   52
 19  \w     33.00 134.00   0.50    0.50    --  107.75 -84.00  87.00  202
 20  \w     37.00  74.00   0.50    0.50    --  107.75 -94.00  90.00   74
 21  \w     81.00 106.00   0.50    0.50    --  107.75 -94.00  90.00   50
 22  \w    -24.00  77.00   0.50    0.50    --   50.71 -84.00  87.00  202
 23  \w     43.00  71.00   0.50    0.50    --  107.75 -77.00 -60.00   56
 24  \w     40.00  65.00   0.50    0.50    --  107.75 -61.00-120.00   50
 25  \w     37.00  68.00   0.50    0.50    --  107.75 -61.00-150.00   62
 26  \w     34.00  87.00   0.50    0.50    --  107.75 -77.00   0.00  106
 27  \w    -28.00  23.00   0.50    0.50    --   50.71 -19.00-120.00  102
 28  \w    -28.00  23.00   0.50    0.50    --   50.71 -19.00  90.00  102
 29  \w     36.00  67.00   0.50    0.50    --  107.75 -61.00 120.00   62
 30  \w     38.00  96.00   0.50    0.50    --  107.75 -77.00 150.00  116
 31  \w     82.00 175.00   0.50    0.50    --  107.75  84.00-152.00  186
 32  \w     78.00 125.00   0.50    0.50    --   50.71  84.00-152.00   94
 33  \w     91.00 138.00   0.50    0.50    --  107.75 111.00  60.00   94
 34  \w     76.00 126.00   0.50    0.50    --   50.71 125.00  60.00  100
 35  \w    -74.00 -29.00   0.50    0.50    -- -100.00  61.00  30.00   90
 36  \w    -54.00 -24.00   0.50    0.50    -- -100.00  45.00 150.00   60
 37  \w    -53.00 -24.00   0.50    0.50    -- -100.00  45.00 120.00   58
 38  \w   -109.00 -23.00   0.50    0.50    -- -100.00 110.00 176.60  172
 39  \w   -108.00 -23.00   0.50    0.50    -- -100.00 108.00 118.39  170
 40  \w   -108.00 -78.00   0.50    0.50    -- -100.00 108.00  33.81   60
 41  \w   -110.00 -24.00   0.50    0.50    -- -100.00 113.00 -74.43  172
 42  \w    -77.00  24.00   0.50    0.50    --  -50.71  84.00-152.00  202
 43  \w   -127.00 -32.00   0.50    0.50    -- -100.00 144.00-152.73  190
 44  \w    -92.00 -67.00   0.50    0.50    -- -100.00 111.00-150.00   50
 45  \w   -100.00 -75.00   0.50    0.50    -- -100.00  84.00-152.00   50
 46  \w   -170.00 -88.00   0.50    0.50    -- -100.00 -45.00-180.00  164
 47  \w   -124.00 -81.00   0.50    0.50    --  -50.71 -77.00 -90.00   86
 48  \w   -124.00 -81.00   0.50    0.50    --  -50.71 -77.00 -60.00   86
 49  \w   -175.00 -87.00   0.50    0.50    -- -100.00 -50.00   9.69  176
 50  \w   -173.00 -85.00   0.50    0.50    -- -100.00 -57.00 158.07  176
 51  \w   -175.00 -83.00   0.50    0.50    -- -100.00 -84.00  87.00  184
 52  \w   -126.00 -81.00   0.50    0.50    --  -50.71-125.00  30.00   90
 53  \w   -126.00 -81.00   0.50    0.50    --  -50.71-125.00-150.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1067362000
_diffrn_orient_matrix_UB_12      -0.0008709000
_diffrn_orient_matrix_UB_13      -0.0894296000
_diffrn_orient_matrix_UB_21      0.0556098000
_diffrn_orient_matrix_UB_22      -0.1228224000
_diffrn_orient_matrix_UB_23      0.0565123000
_diffrn_orient_matrix_UB_31      -0.0575138000
_diffrn_orient_matrix_UB_32      -0.0279363000
_diffrn_orient_matrix_UB_33      -0.0568088000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            45880
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.502
_diffrn_reflns_theta_min         3.445
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.983
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_description       block
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.961
_refine_diff_density_min         -1.588
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         8865
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0744
_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^)+(0.0723P)^2^+10.1038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1838
_refine_ls_wR_factor_ref         0.1848
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8506
_reflns_number_total             8865
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00848c2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1566968--1566970.cif.'
_cod_database_code               1566968
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu O C N F S H'
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.796
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F8A-C36A \\sim F6A-C36A \\sim F7A-C36A
 with sigma of 0.0001
 F8-C36 \\sim F7-C36 \\sim F6-C36
 with sigma of 0.0001
3. Uiso/Uaniso restraints and constraints
C36 \\sim S2: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
S2 \\sim O3: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C36A \\sim S2A: within 2A with sigma of 0.0001 and sigma for terminal atoms of
0.0002 within 2A
Uanis(F7A) = Uanis(F7)
4. Rigid body (RIGU) restrains
 C36, F6, F7, F8
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 F4A, C35, F3A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(H39)=Sof(F10A)=1-FVAR(1)
 Sof(F10)=Sof(H41)=FVAR(1)
 Sof(S2A)=Sof(S1A)=Sof(N7A)=Sof(O3A)=Sof(O1A)=Sof(C36A)=Sof(F7A)=Sof(F6A)=
 Sof(F8A)=Sof(O2A)=Sof(F3A)=Sof(F4A)=1-FVAR(2)
 Sof(S1)=Sof(S2)=Sof(N7)=Sof(O2)=Sof(O3)=Sof(F5)=Sof(O1)=Sof(C36)=Sof(F8)=
 Sof(F6)=Sof(F7)=Sof(F3)=FVAR(2)
 Sof(O5)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C33A)=Sof(H33D)=Sof(H33E)=
 Sof(H33F)=1-FVAR(3)
 Sof(O5A)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34)=Sof(H34A)=Sof(H34B)=
 Sof(H34C)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 C25(H25), C6(H6), C2(H2), C11(H11), C3(H3), C5(H5), C27(H27), C30(H30),
 C12(H12), C22(H22), C29(H29), C24(H24), C28(H28), C16(H16), C23(H23), C17(H17),
  C19(H19), C37(H37), C42(H42), C13(H13), C18(H18), C14(H14), C41(H41),
 C38(H38), C39(H39)
6.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C34A(H34D,H34E,
 H34F), C33A(H33D,H33E,H33F)
;
_shelx_res_checksum              87293
_shelx_hkl_checksum              53880
_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 1.695
_oxdiff_exptl_absorpt_empirical_full_min 0.684