Acridine-based copper(I) PNP pincer complexes: catalysts for alkyne hydroboration and borylation of aryl halides.
Olding, Angus; Lucas, Nigel T.; Ho, Curtis C.; Bissember, Alex C.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 4471–4478; doi:10.1039/d3dt04269c

data_7715123
_publ_section_title
;
 Acridine-based copper(I) PNP pincer complexes: catalysts for alkyne
 hydroboration and borylation of aryl halides.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4471
_journal_page_last               4478
_journal_paper_doi               10.1039/d3dt04269c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C41 H58 Cu N2 P2, F6 P, C2 H3 N'
_chemical_formula_sum            'C43 H58 Cu F6 N3 P3'
_chemical_formula_weight         887.37
_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             2023-01-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-12-16 deposited with the CCDC.	2024-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.071(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7292(5)
_cell_length_b                   14.5532(5)
_cell_length_c                   23.7256(8)
_cell_measurement_reflns_used    5137
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.9140
_cell_measurement_theta_min      4.6430
_cell_volume                     4351.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3449
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.969
_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   -130.00  46.00   1.00    2.50    --  -41.92   0.00 -90.00  176
  2  \w     17.00  74.00   1.00    2.50    --   41.92 -99.00  30.00   57
  3  \w     41.00  96.00   1.00   10.00    --  104.32 -95.00 120.00   55
  4  \w    116.00 146.00   1.00   10.00    --  104.32  77.00-180.00   30
  5  \w     82.00 177.00   1.00   10.00    --  104.32  61.00 120.00   95
  6  \w    107.00 178.00   1.00   10.00    --  104.32  77.00 -30.00   71
  7  \w     34.00 129.00   1.00   10.00    --  104.32 -45.00 -30.00   95
  8  \w     44.00  80.00   1.00   10.00    --  104.32 -45.00-180.00   36
  9  \w     80.00 124.00   1.00   10.00    --  104.32  61.00 150.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0350990000
_diffrn_orient_matrix_UB_12      0.0676490000
_diffrn_orient_matrix_UB_13      -0.0436945000
_diffrn_orient_matrix_UB_21      0.0893569000
_diffrn_orient_matrix_UB_22      0.0355288000
_diffrn_orient_matrix_UB_23      0.0453737000
_diffrn_orient_matrix_UB_31      0.0756219000
_diffrn_orient_matrix_UB_32      -0.0732023000
_diffrn_orient_matrix_UB_33      -0.0184030000
_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  0.0326
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16859
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         72.588
_diffrn_reflns_theta_min         3.573
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.254
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       plate
_exptl_crystal_F_000             1860
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.355
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         8376
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0812
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1921P)^2^+0.1150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2382
_refine_ls_wR_factor_ref         0.2603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5997
_reflns_number_total             8376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04269c2.cif
_cod_data_source_block           compound_1a
_cod_depositor_comments
'Adding full bibliography for 7715123--7715127.cif.'
_cod_database_code               7715123
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C39 H55 Cu1 F6 N1 P3'
_chemical_oxdiff_usercomment     'M616 NTL acb_AO-7-133A'
_shelx_estimated_absorpt_t_max   0.806
_shelx_estimated_absorpt_t_min   0.581
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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 Ternary CH refined with riding coordinates:
 C21(H21), C27(H27), C41(H41), C47(H47)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C25(H25A,H25B), C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C42(H42A,H42B), C43(H43A,H43B),
  C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C48(H48A,H48B), C49(H49A,
 H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8)
2.d Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C92(H92A,H92B,H92C)
;
_shelx_res_checksum              32159
_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 1.397
_oxdiff_exptl_absorpt_empirical_full_min 0.748