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_1566969
_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
'C36 H24 B Cu2 F2 N6 O2, C2 F6 N O4 S2, 0.75[C6H4F2]'
_chemical_formula_sum            'C38 H24 B Cu2 F8 N7 O6 S2'
_chemical_formula_weight         1028.65
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-12-06
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2021-12-23 deposited with the CCDC.	2022-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.6180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.31060(10)
_cell_length_b                   22.6847(3)
_cell_length_c                   15.3728(2)
_cell_measurement_reflns_used    28322
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      78.4810
_cell_measurement_theta_min      3.0110
_cell_volume                     4424.05(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.15
_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 0.997
_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     99.00 173.00   0.50    0.50    --  107.75  45.00  30.00  148
  2  \w    134.00 174.00   0.50    0.50    --  107.75  15.00-120.00   80
  3  \w     98.00 125.00   0.50    0.50    --  107.75  15.00-120.00   54
  4  \w     93.00 122.00   0.50    0.50    --   50.71  77.00  60.00   58
  5  \w     82.00 124.00   0.50    0.50    --   50.71  77.00  90.00   84
  6  \w    -22.00  22.00   0.50    0.50    --  -50.71  19.00 -60.00   88
  7  \w    -54.00 -29.00   0.50    0.50    -- -100.00  45.00-180.00   50
  8  \w    -51.00 -25.00   0.50    0.50    -- -100.00  45.00-150.00   52
  9  \w    -54.00 -29.00   0.50    0.50    -- -100.00  45.00   0.00   50
 10  \w    -54.00 -28.00   0.50    0.50    -- -100.00  45.00 150.00   52
 11  \w    -54.00 -29.00   0.50    0.50    -- -100.00  45.00 120.00   50
 12  \w    -86.00   1.00   0.50    0.50    --  -50.71 102.00  29.00  174
 13  \w   -107.00 -23.00   0.50    0.50    -- -100.00 102.00  29.00  168
 14  \w   -170.00-110.00   0.50    0.50    -- -100.00-102.00 -72.00  120
 15  \w   -123.00 -85.00   0.50    0.50    --  -50.71 -77.00 -60.00   76
 16  \w   -121.00 -82.00   0.50    0.50    --  -50.71 -77.00 150.00   78
 17  \w    -21.00  63.00   0.50    0.50    --   50.71 -57.00 -30.00  168
 18  \w     42.00 102.00   0.50    0.50    --  107.75 -77.00-150.00  120
 19  \w     40.00  70.00   0.50    0.50    --  107.75 -77.00-180.00   60
 20  \w     43.00 102.00   0.50    0.50    --  107.75 -77.00 -60.00  118
 21  \w     39.00  65.00   0.50    0.50    --  107.75 -61.00 -60.00   52
 22  \w     38.00  65.00   0.50    0.50    --  107.75 -61.00  90.00   54
 23  \w     38.00  63.00   0.50    0.50    --  107.75 -61.00 120.00   50
 24  \w     36.00  79.00   0.50    0.50    --  107.75 -77.00 150.00   86
 25  \w     36.00  62.00   0.50    0.50    --  107.75 -61.00 150.00   52
 26  \w     38.00  65.00   0.50    0.50    --  107.75 -61.00  60.00   54
 27  \w     40.00  66.00   0.50    0.50    --  107.75 -61.00   0.00   52
 28  \w     37.00  66.00   0.50    0.50    --  107.75 -61.00 -30.00   58
 29  \w     36.00  68.00   0.50    0.50    --  107.75 -61.00-150.00   64
 30  \w     40.00  65.00   0.50    0.50    --  107.75 -61.00-180.00   50
 31  \w    106.00 131.00   0.50    0.50    --  107.75 102.00  29.00   50
 32  \w     32.00 100.00   0.50    0.50    --  107.75 -94.00 -60.00  136
 33  \w     83.00 108.00   0.50    0.50    --  107.75-102.00 -72.00   50
 34  \w     33.00  59.00   0.50    0.50    --  107.75-102.00 -72.00   52
 35  \w     -7.00  86.00   0.50    0.50    --   50.71-102.00 -72.00  186
 36  \w     58.00 103.00   0.50    0.50    --  107.75-111.00  30.00   90
 37  \w     35.00 103.00   0.50    0.50    --  107.75 -94.00  30.00  136
;
_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      -0.0480477000
_diffrn_orient_matrix_UB_12      -0.0605331000
_diffrn_orient_matrix_UB_13      0.0093439000
_diffrn_orient_matrix_UB_21      -0.0365563000
_diffrn_orient_matrix_UB_22      0.0238475000
_diffrn_orient_matrix_UB_23      0.0792849000
_diffrn_orient_matrix_UB_31      -0.1053999000
_diffrn_orient_matrix_UB_32      0.0193725000
_diffrn_orient_matrix_UB_33      -0.0684601000
_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  0.0393
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            48153
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.504
_diffrn_reflns_theta_min         3.591
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.837
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'yellow orange'
_exptl_crystal_colour_modifier   yellow
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.902
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         9029
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0830
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+25.7628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1948
_refine_ls_wR_factor_ref         0.1964
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8350
_reflns_number_total             9029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00848c2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 1566968--1566970.cif.'
_cod_database_code               1566969
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu B C N O S F H'
_shelx_estimated_absorpt_t_max   0.826
_shelx_estimated_absorpt_t_min   0.526
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F6-F7 \\sim F7-F8
 with sigma of 0.00001
 F8-C38 \\sim F7-C38 \\sim F6-C38
 with sigma of 0.00001
 F8A-F7A \\sim F7A-F6A
 with sigma of 0.00001
 F8A-C38A \\sim F7A-C38A \\sim F6A-C38A
 with sigma of 0.00001
 F4-C37 \\sim F3-C37 \\sim F5-C37
 with sigma of 0.0001
 F4-F5 \\sim F5-F3
 with sigma of 0.0001
3. Uiso/Uaniso restraints and constraints
Uanis(C37A) = Uanis(C37)
4. Rigid body (RIGU) restrains
 C37A, F5A, F4A
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 F8, C38, F7, F6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C38A, F6A, F7A, F8A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 F4, F5, C37, F3
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
5. Others
 Sof(S1A)=Sof(S2A)=Sof(N7A)=Sof(O4A)=Sof(O6A)=Sof(F7)=Sof(F6)=Sof(F8)=Sof(C38)=
 Sof(F4A)=Sof(F5A)=Sof(C37A)=1-FVAR(1)
 Sof(S1)=Sof(S2)=Sof(F5)=Sof(F4)=Sof(N7)=Sof(O4)=Sof(C37)=Sof(F7A)=Sof(F6A)=
 Sof(F8A)=Sof(O6)=Sof(C38A)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C29(H29), C3(H3), C5(H5), C25(H25), C27(H27), C30(H30), C19(H19),
 C28(H28), C22(H22), C2(H2), C17(H17), C32(H32), C16(H16), C18(H18), C24(H24),
 C33(H33), C14(H14), C23(H23), C35(H35), C34(H34), C13(H13), C11(H11), C12(H12)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 176 electrons were 
found in a volume of 492A^3 in 1 void per unit cell. 
This is consistent with the presence of 
0.75[C6H4F2] per Asymmetric Unit 
which account for 174 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              7536
_shelx_hkl_checksum              65501
_shelx_fab_checksum              32940
_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 1.653
_oxdiff_exptl_absorpt_empirical_full_min 0.698