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_7701962
_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     dual
_audit_creation_date             2019-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-17 deposited with the CCDC.	2019-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                62.868(2)
_cell_angle_beta                 73.374(2)
_cell_angle_gamma                78.798(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8853(2)
_cell_length_b                   13.5954(3)
_cell_length_c                   14.8780(2)
_cell_measurement_reflns_used    14823
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.9360
_cell_measurement_theta_min      4.6560
_cell_volume                     1700.32(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.47a (Rigaku OD, 2019)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_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    -84.00  94.00   0.50    1.00    --    5.00   0.00-180.00  356
  2  \w    -84.00  94.00   0.50    1.00    --    5.00  59.00 -30.00  356
  3  \w   -179.00  -1.00   0.50    3.00    --  -90.00  59.00 169.19  356
  4  \w   -179.00  -1.00   0.50    3.00    --  -90.00  58.00-123.64  356
  5  \w   -179.00  -1.00   0.50    3.00    --  -90.00  56.00 -38.12  356
  6  \w   -179.00  -1.00   0.50    3.00    --  -90.00  59.00  90.12  356
  7  \w   -179.00  -1.00   0.50    3.00    --  -90.00  39.00  30.00  356
  8  \w   -142.00 -17.00   0.50    3.00    --  -90.00  59.00  28.33  250
  9  \w   -179.00  -1.00   0.50    3.00    --  -90.00  55.00 110.46  356
 10  \w   -142.00 -17.00   0.50    3.00    --  -90.00  59.00  28.33  250
 11  \w   -137.00 -84.00   0.50    3.00    --  -90.00  49.00 -90.00  106
 12  \w    -42.00  -2.00   0.50    3.00    --  -90.00  49.00 -90.00   80
 13  \w   -179.00 -88.00   0.50    3.00    --  -90.00  10.00-120.00  182
 14  \w    -84.00  -2.00   0.50    3.00    --  -90.00  10.00-120.00  164
 15  \w    -88.00 -62.00   0.50    3.00    --  -90.00  59.00 169.19   52
 16  \w   -178.00-131.00   0.50    3.00    --  -90.00  58.00 -19.30   94
 17  \w   -177.00-152.00   0.50    3.00    --  -90.00  58.00-140.40   50
 18  \w    -55.00  -1.00   0.50    3.00    --  -90.00  58.00-140.40  108
 19  \w   -177.00  -3.00   0.50    3.00    --  -90.00  59.00-151.66  348
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter \c goniometer'
_diffrn_measurement_device_type  Dot_HyPix
_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      -0.0253185000
_diffrn_orient_matrix_UB_12      0.0007394000
_diffrn_orient_matrix_UB_13      0.1068268000
_diffrn_orient_matrix_UB_21      0.0101182000
_diffrn_orient_matrix_UB_22      -0.1276745000
_diffrn_orient_matrix_UB_23      0.0516766000
_diffrn_orient_matrix_UB_31      0.1607279000
_diffrn_orient_matrix_UB_32      -0.0016223000
_diffrn_orient_matrix_UB_33      -0.0138019000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19916
_diffrn_reflns_point_group_measured_fraction_full 0.858
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         3.427
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.47a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       Rod
_exptl_crystal_F_000             654
_exptl_crystal_recrystallization_method 'as supplied'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.030(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         19916
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0645
_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^)+(0.1427P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1669
_refine_ls_wR_factor_ref         0.1711
_reflns_Friedel_coverage         0.725
_reflns_Friedel_fraction_full    0.723
_reflns_Friedel_fraction_max     0.717
_reflns_number_gt                17893
_reflns_number_total             19916
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9832\% 
 around [0.00 0.89 0.45] (reciprocal) or [-0.28 0.96 0.05] (direct)
;
_cod_data_source_file            c9dt04146j2.cif
_cod_data_source_block           2019ncs0339z_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7701961--7701962.cif.'
_cod_database_code               7701962
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C71 H103 Cu2 N4 O4 '
_chemical_oxdiff_usercomment     SS779-MD065
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.771
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8241(7)
 0.1759(7)
2. 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
3.a Ternary CH refined with riding coordinates:
 C1(H1), C6(H6), C101(H101), C106(H106)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C102(H10A,H10B),
 C103(H10C,H10D), C104(H10E,H10F), C105(H10G,H10H)
3.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C11(H11), C22(H22), C24(H24), C26(H26), C107(H107),
 C109(H109), C111(H111), C122(H122), C124(H124), C126(H126)
3.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C115(H11A,H11B,H11C), C116(H11D,H11E,H11F), C117(H11G,
 H11H,H11I), C119(H11J,H11K,H11L), C120(H12A,H12B,H12C), C121(H12D,H12E,H12F),
 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              96243
_olex2_date_sample_data_collection 2019-04-10
_olex2_date_sample_submission    2019-04-10
_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 SS779-MD065
_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 2.245
_oxdiff_exptl_absorpt_empirical_full_min 0.597
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2