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_7708006
_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         'C24 H32 Cu N2 O2'
_chemical_formula_sum            'C24 H32 Cu N2 O2'
_chemical_formula_weight         444.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6031(4)
_cell_length_b                   16.8736(6)
_cell_length_c                   18.7628(8)
_cell_measurement_reflns_used    3093
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      71.4300
_cell_measurement_theta_min      5.1980
_cell_volume                     2407.11(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.985
_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      9.00 108.00   1.00   40.00    --   37.81  19.00   0.00   99
  2  \w     20.00 106.00   1.00   40.00    --   37.81  38.00 150.00   86
  3  \w     88.00 174.00   1.00   70.00    --  107.00 111.00 120.00   86
  4  \w     85.00 172.00   1.00   70.00    --  107.00  77.00  60.00   87
  5  \w     94.00 172.00   1.00   70.00    --  107.00  61.00-150.00   78
  6  \w     53.00  84.00   1.00   70.00    --  107.00-111.00 -30.00   31
  7  \w     40.00 125.00   1.00   70.00    --  107.00 -61.00  60.00   85
;
_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      -0.0068677000
_diffrn_orient_matrix_UB_12      -0.0913379000
_diffrn_orient_matrix_UB_13      -0.0017528000
_diffrn_orient_matrix_UB_21      0.1212733000
_diffrn_orient_matrix_UB_22      -0.0002019000
_diffrn_orient_matrix_UB_23      -0.0659397000
_diffrn_orient_matrix_UB_31      0.1619372000
_diffrn_orient_matrix_UB_32      -0.0036491000
_diffrn_orient_matrix_UB_33      0.0488639000
_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  0.0225
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6887
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.76
_diffrn_reflns_theta_min         3.53
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.430
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       plate
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 1617 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.32(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4518
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0486P)^2^+0.4559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0937
_reflns_Friedel_coverage         0.709
_reflns_Friedel_fraction_full    0.972
_reflns_Friedel_fraction_max     0.931
_reflns_number_gt                4172
_reflns_number_total             4518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01950c2.cif
_cod_data_source_block           jd441
_cod_depositor_comments
'Adding full bibliography for 7708002--7708009.cif.'
_cod_original_cell_volume        2407.10(17)
_cod_database_code               7708006
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Cu1 H22 N2 O2'
_diffrn_oxdiff_ac3_digest_frames
;
01564b7a393ef74e74450cae676a4ac1ee00027e0ee
;
_diffrn_oxdiff_ac3_digest_hkl
;
01c136e980b179fa9d5a24f4d1f7ea8f4c62ae
;
_reflns_odcompleteness_completeness 99.36
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 H1-N1
 0.98 with sigma of 0.02
2.a Ternary CH refined with riding coordinates:
 N2(H2), C12(H12), C17(H17)
2.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,
 H16B), C18(H18A,H18B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4), C20(H20), C21(H21), C22(H22), C23(H23)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_olex2_date_sample_data_collection 2020-07-20
_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 1.316
_oxdiff_exptl_absorpt_empirical_full_min 0.731