Breaking the symmetry: <i>C</i><sub>1</sub>-salans with (N-H) backbones.
Devonport, Jack; Spencer, John; Kostakis, George E.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 12069–12073; doi:10.1039/d1dt01950c

data_7708009
_publ_section_title
;
 Breaking the symmetry: <i>C</i><sub>1</sub>-salans with (N-H) backbones.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12069
_journal_page_last               12073
_journal_paper_doi               10.1039/d1dt01950c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C40 H46 Cu2 F2 N4 O4'
_chemical_formula_sum            'C40 H46 Cu2 F2 N4 O4'
_chemical_formula_weight         811.89
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-26 deposited with the CCDC.	2021-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                79.623(5)
_cell_angle_beta                 89.276(4)
_cell_angle_gamma                67.850(5)
_cell_formula_units_Z            1
_cell_length_a                   9.0899(5)
_cell_length_b                   9.3275(6)
_cell_length_c                   10.9768(5)
_cell_measurement_reflns_used    7232
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.7800
_cell_measurement_theta_min      5.1730
_cell_volume                     846.33(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (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 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.981
_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    -25.00  82.00   1.00    5.00    --    0.00  20.00   0.00  107
  2  \w   -104.00  69.00   1.00    5.00    --  -20.00  58.00 -26.82  173
  3  \w    -65.00  41.00   1.00   18.00    --  -48.00  60.00-120.76  106
  4  \w      7.00  35.00   1.00   18.00    --  -52.00  41.00  69.88   28
  5  \w    -21.00  37.00   1.00   18.00    --  -52.00  55.00 135.57   58
  6  \w      1.00  29.00   1.00   18.00    --  -60.00  48.00 161.59   28
  7  \w   -123.00 -79.00   1.00   18.00    --  -60.00  48.00 161.59   44
  8  \w     -3.00  25.00   1.00   18.00    --  -64.00  57.00  24.14   28
  9  \w     -9.00  25.00   1.00   18.00    --  -64.00  50.00  70.79   34
 10  \w   -135.00-107.00   1.00   18.00    --  -64.00  57.00  24.14   28
 11  \w    -16.00  20.00   1.00   18.00    --  -68.00  53.00 -16.41   36
 12  \w    -29.00   0.00   1.00   18.00    --  -89.00  58.00  64.61   29
 13  \w   -101.00   0.00   1.00   18.00    --  -89.00  54.00 -39.62  101
 14  \w   -140.00   0.00   1.00   18.00    --  -89.00  59.00 -68.31  140
 15  \w    -66.00   0.00   1.00   18.00    --  -89.00  60.00 -86.75   66
 16  \w    -29.00   0.00   1.00   18.00    --  -89.00  57.00  -3.76   29
 17  \w    -98.00 -70.00   1.00   18.00    --  -89.00  57.00  -3.76   28
 18  \w   -106.00 -77.00   1.00   18.00    --  -89.00  60.00 -86.75   29
 19  \w   -177.00   0.00   1.00   18.00    --  -89.00  59.00  83.76  177
 20  \w   -178.00-140.00   1.00   18.00    --  -89.00  60.00 -86.75   38
 21  \w    -25.00   0.00   1.00   18.00    --  -89.00  60.00 -50.06   25
 22  \w   -128.00  -1.00   1.00   18.00    --  -89.00  58.00 134.22  127
 23  \w   -117.00 -89.00   1.00   18.00    --  -89.00  57.00  48.81   28
 24  \w   -161.00-132.00   1.00   18.00    --  -89.00  60.00 -50.06   29
 25  \w   -119.00   0.00   1.00   18.00    --  -89.00  59.00 -18.24  119
 26  \w    -90.00 -45.00   1.00   18.00    --  -89.00  58.00  64.61   45
 27  \w    -28.00   0.00   1.00   18.00    --  -89.00  56.00-151.72   28
 28  \w    -93.00 -60.00   1.00   18.00    --  -89.00  59.00 111.86   33
 29  \w    -56.00   0.00   1.00   18.00    --  -89.00  59.00 111.86   56
 30  \w   -173.00-134.00   1.00   18.00    --  -89.00  60.00-170.46   39
 31  \w    -29.00   0.00   1.00   18.00    --  -89.00  50.00 150.00   29
 32  \w    -99.00 -31.00   1.00   18.00    --  -89.00  56.00-151.72   68
 33  \w    -97.00 -48.00   1.00   18.00    --  -89.00  50.00 150.00   49
 34  \w   -125.00   0.00   1.00   18.00    --  -89.00  58.00 173.83  125
 35  \w   -129.00   0.00   1.00   18.00    --  -89.00  60.00  21.49  129
 36  \w   -148.00  -1.00   1.00   18.00    --  -89.00  55.00-111.95  147
 37  \w   -103.00 -47.00   1.00   18.00    --  -89.00  58.00  35.34   56
 38  \w    -25.00   0.00   1.00   18.00    --  -89.00  58.00  35.34   25
 39  \w    -30.00   0.00   1.00   18.00    --  -89.00  60.00-170.46   30
 40  \w    -66.00 -36.00   1.00   18.00    --  -89.00  60.00-170.46   30
 41  \w    -60.00  -4.00   1.00   18.00    --  -89.00  57.00  48.81   56
 42  \w   -114.00 -59.00   1.00   18.00    --  -89.00  59.00 106.82   55
 43  \w    -25.00   0.00   1.00   18.00    --  -89.00  59.00 106.82   25
 44  \w   -136.00-108.00   1.00   18.00    --  -89.00  57.00-131.74   28
 45  \w    -87.00   0.00   1.00   18.00    --  -89.00  57.00-131.74   87
 46  \w   -167.00-138.00   1.00   18.00    --  -89.00  60.00  21.49   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1779631000
_diffrn_orient_matrix_UB_12      -0.0630351000
_diffrn_orient_matrix_UB_13      -0.0257235000
_diffrn_orient_matrix_UB_21      0.0363941000
_diffrn_orient_matrix_UB_22      -0.1214617000
_diffrn_orient_matrix_UB_23      0.1221988000
_diffrn_orient_matrix_UB_31      -0.0247347000
_diffrn_orient_matrix_UB_32      -0.1193968000
_diffrn_orient_matrix_UB_33      -0.0695615000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1099
_diffrn_reflns_av_unetI/netI     0.0659
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17272
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.054
_diffrn_reflns_theta_min         5.214
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.064
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       plate
_exptl_crystal_F_000             422
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.892
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3029
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0811
_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^)+(0.0928P)^2^+4.2596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1877
_refine_ls_wR_factor_ref         0.1933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2703
_reflns_number_total             3029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01950c2.cif
_cod_data_source_block           jd515
_cod_depositor_comments
'Adding full bibliography for 7708002--7708009.cif.'
_cod_database_code               7708009
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C38 H50 Cu1 N2 O2 F1 '
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.960
_reflns_odcompleteness_completeness 99.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), C8(H8), C13(H13)
1.b Secondary CH2 refined with riding coordinates:
 C7(H7B,H7A), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C14(H14A,H14B)
1.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C5(H5), C16(H16), C17(H17), C18(H18), C19(H19)
;
_shelx_res_checksum              10339
_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 1.715
_oxdiff_exptl_absorpt_empirical_full_min 0.242