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_7708008
_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         'C28 H36 Cu N2 O2'
_chemical_formula_sum            'C28 H36 Cu N2 O2'
_chemical_formula_weight         496.13
_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                86.427(6)
_cell_angle_beta                 78.259(5)
_cell_angle_gamma                76.948(5)
_cell_formula_units_Z            2
_cell_length_a                   9.4670(5)
_cell_length_b                   10.0851(7)
_cell_length_c                   13.7290(9)
_cell_measurement_reflns_used    3447
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      71.7860
_cell_measurement_theta_min      4.5060
_cell_volume                     1250.02(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.96a (Rigaku OD, 2021)'
_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)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.957
_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    -15.00  72.00   1.00    1.00    --   37.91-101.00 -22.00   87
  2  \w    135.00 174.00   1.00    1.00    --  107.00 101.00  81.00   39
  3  \w     20.00 105.00   1.00    1.00    --   37.91  38.00 -90.00   85
  4  \w     41.00 108.00   1.00    1.00    --   37.91 178.00 120.00   67
  5  \w     27.00 104.00   1.00    1.00    --   37.91  57.00 120.00   77
  6  \w      5.00  76.00   1.00    1.00    --   37.91 -99.00-180.00   71
  7  \w     55.00  97.00   1.00    1.00    --   37.91  19.00  30.00   42
  8  \w     71.00 106.00   1.00    1.00    --  107.00 -77.00 -60.00   35
  9  \w     37.00 127.00   1.00    1.00    --  107.00 -30.00 -60.00   90
 10  \w     75.00 102.00   1.00    1.00    --  107.00 -77.00   0.00   27
 11  \w     39.00  84.00   1.00    1.00    --  107.00-111.00 -90.00   45
 12  \w     41.00  83.00   1.00    1.00    --  107.00-111.00 -60.00   42
 13  \w     48.00  73.00   1.00    1.00    --  107.00 -45.00  30.00   25
 14  \w     86.00 117.00   1.00    1.00    --  107.00 -45.00  30.00   31
 15  \w     41.00 113.00   1.00    1.00    --  107.00 -77.00 150.00   72
 16  \w     82.00 114.00   1.00    1.00    --  107.00 -77.00-150.00   32
 17  \w     67.00 112.00   1.00    1.00    --  107.00 -77.00  60.00   45
 18  \w     90.00 175.00   1.00    1.00    --  107.00  45.00 120.00   85
 19  \w     44.00 110.00   1.00    1.00    --  107.00 -15.00-180.00   66
 20  \w     37.00  62.00   1.00    1.00    --  107.00-111.00-120.00   25
 21  \w     44.00  71.00   1.00    1.00    --  107.00 -77.00   0.00   27
 22  \w     56.00  84.00   1.00    1.00    --  107.00-111.00  60.00   28
 23  \w     37.00 136.00   1.00    1.00    --  107.00 -15.00  90.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0370887000
_diffrn_orient_matrix_UB_12      0.0763881000
_diffrn_orient_matrix_UB_13      -0.0954504000
_diffrn_orient_matrix_UB_21      0.0333317000
_diffrn_orient_matrix_UB_22      -0.1366658000
_diffrn_orient_matrix_UB_23      -0.0534941000
_diffrn_orient_matrix_UB_31      -0.1628487000
_diffrn_orient_matrix_UB_32      -0.0095920000
_diffrn_orient_matrix_UB_33      0.0341403000
_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  0.0320
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8028
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.893
_diffrn_reflns_theta_min         4.501
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.434
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.96a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       block
_exptl_crystal_F_000             526
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.274
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4696
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+0.9922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1182
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3876
_reflns_number_total             4696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01950c2.cif
_cod_data_source_block           jd837_auto
_cod_depositor_comments
'Adding full bibliography for 7708002--7708009.cif.'
_cod_database_code               7708008
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cu H C N O '
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.870
_reflns_odcompleteness_completeness 98.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C8(H8), C13(H13)
1.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B)
1.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19)
1.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)
;
_shelx_res_checksum              33656
_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 1.405
_oxdiff_exptl_absorpt_empirical_full_min 0.814