Shedding light on the use of Cu(ii)-salen complexes in the A<sup>3</sup> coupling reaction.
Sampani, Stavroula I.; Zdorichenko, Victor; Danopoulou, Marianna; Leech, Matthew C.; Lam, Kevin; Abdul-Sada, Alaa; Cox, Brian; Tizzard, Graham J.; Coles, Simon J.; Tsipis, Athanassios; Kostakis, George E.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 289–299; doi:10.1039/c9dt04146j

data_7701961
_publ_section_title
;
 Shedding light on the use of Cu(ii)-salen complexes in the A<sup>3</sup>
 coupling reaction.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              289
_journal_page_last               299
_journal_paper_doi               10.1039/c9dt04146j
_journal_volume                  49
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H52 Cu N2 O2'
_chemical_formula_sum            'C36 H52 Cu N2 O2'
_chemical_formula_weight         608.33
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-03-15
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2019-09-17 deposited with the CCDC.	2019-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                62.868(4)
_cell_angle_beta                 73.368(3)
_cell_angle_gamma                78.772(3)
_cell_formula_units_Z            2
_cell_length_a                   9.8740(4)
_cell_length_b                   13.5904(5)
_cell_length_c                   14.8719(6)
_cell_measurement_reflns_used    6286
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.2880
_cell_measurement_theta_min      3.1150
_cell_volume                     1696.94(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.998
_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    -34.00  80.00   1.00   20.00    --   -9.60  38.00  30.00  114
  2  \w    -99.00  15.00   1.00   20.00    --   -9.60 -38.00  90.00  114
  3  \w    -99.00  20.00   1.00   20.00    --   -9.60 -57.00  60.00  119
  4  \w    -34.00  80.00   1.00   20.00    --   -9.60  38.00-120.00  114
  5  \w    -96.00  18.00   1.00   20.00    --   -9.60 -72.00 -90.00  114
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0143107000
_diffrn_orient_matrix_UB_12      0.0565496000
_diffrn_orient_matrix_UB_13      -0.0299928000
_diffrn_orient_matrix_UB_21      0.0700182000
_diffrn_orient_matrix_UB_22      -0.0132088000
_diffrn_orient_matrix_UB_23      0.0079233000
_diffrn_orient_matrix_UB_31      0.0233534000
_diffrn_orient_matrix_UB_32      -0.0092990000
_diffrn_orient_matrix_UB_33      -0.0454367000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.1274
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31262
_diffrn_reflns_point_group_measured_fraction_full 0.945
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.950
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.9g (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale brown'
_exptl_crystal_colour_modifier   pale
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_description       rod
_exptl_crystal_F_000             654
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 3116 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         14276
_refine_ls_number_restraints     747
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.0655
_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^)+(0.0339P)^2^+0.6439P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1276
_reflns_Friedel_coverage         0.838
_reflns_Friedel_fraction_full    0.892
_reflns_Friedel_fraction_max     0.836
_reflns_number_gt                9806
_reflns_number_total             14276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04146j2.cif
_cod_data_source_block           2017ncs0064za
_cod_depositor_comments
'Adding full bibliography for 7701961--7701962.cif.'
_cod_database_code               7701961
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C36 H54 N2 O2 Cu'
_chemical_oxdiff_usercomment     SS269
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 C8(H8), C13(H13), C108(H108), C113(H113)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C109(H10C,H10D),
 C110(H11C,H11D), C111(H11E,H11F), C112(H11G,H11H)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C14(H14), C16(H16), C18(H18), C103(H103), C105(H105),
 C107(H107), C114(H114), C116(H116), C118(H118)
3.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C122(H12C,H12D,H12E), C123(H12F,H12G,H12H), C124(H12I,
 H12J,H12K), C126(H12L,H12M,H12N), C127(H12O,H12P,H12Q), C128(H12R,H12S,H12T),
 C130(H13A,H13B,H13C), C131(H13D,H13E,H13F), C132(H13G,H13H,H13I), C134(H13J,
 H13K,H13L), C135(H13M,H13N,H13O), C136(H13P,H13Q,H13R)
;
_shelx_res_checksum              18384
_olex2_date_sample_data_collection 2017-03-20
_olex2_date_sample_submission    2017-02-16
_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 SS269
_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 1.536
_oxdiff_exptl_absorpt_empirical_full_min 0.640