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_7708007
_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         'C17 H22 Cu N2 O4'
_chemical_formula_sum            'C17 H22 Cu N2 O4'
_chemical_formula_weight         381.90
_space_group_crystal_system      orthorhombic
_space_group_IT_number           45
_space_group_name_Hall           'I 2 -2c'
_space_group_name_H-M_alt        'I b a 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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            8
_cell_length_a                   25.4875(6)
_cell_length_b                   14.8482(3)
_cell_length_c                   8.4815(2)
_cell_measurement_reflns_used    4502
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      68.5670
_cell_measurement_theta_min      3.4870
_cell_volume                     3209.77(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (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 2014/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.992
_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    -89.00  89.00   0.50    2.50    --    0.00  39.00 -30.00  356
  2  \w   -179.00  -1.00   0.50   10.00    --  -90.00  59.00 125.89  356
  3  \w   -179.00  -1.00   0.50   10.00    --  -90.00  59.00 -32.78  356
  4  \w   -179.00  -1.00   0.50   10.00    --  -90.00  53.00-100.88  356
  5  \w   -179.00  -1.00   0.50   10.00    --  -90.00  59.00-164.64  356
  6  \w   -152.00 -38.00   0.50   10.00    --  -90.00  38.00 -69.10  228
  7  \w    -46.00 -20.00   0.50   10.00    --  -90.00  59.00 -26.49   52
  8  \w   -163.00 -53.00   0.50   10.00    --  -90.00  59.00 -26.49  220
;
_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      -0.0003026000
_diffrn_orient_matrix_UB_12      -0.1035338000
_diffrn_orient_matrix_UB_13      -0.0116929000
_diffrn_orient_matrix_UB_21      0.0601774000
_diffrn_orient_matrix_UB_22      0.0001277000
_diffrn_orient_matrix_UB_23      -0.0171374000
_diffrn_orient_matrix_UB_31      0.0056598000
_diffrn_orient_matrix_UB_32      -0.0067215000
_diffrn_orient_matrix_UB_33      0.1804535000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14210
_diffrn_reflns_point_group_measured_fraction_full 0.887
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.111
_diffrn_reflns_theta_min         5.960
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.137
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (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    1.581
_exptl_crystal_description       plate
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.423
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 938 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         2673
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0719P)^2^+6.0492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1246
_reflns_Friedel_coverage         0.653
_reflns_Friedel_fraction_full    0.764
_reflns_Friedel_fraction_max     0.748
_reflns_number_gt                2574
_reflns_number_total             2673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01950c2.cif
_cod_data_source_block           2019ncsx0287r1z
_cod_depositor_comments
'Adding full bibliography for 7708002--7708009.cif.'
_cod_database_code               7708007
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'C17 H22 Cu N2 O4'
_chemical_oxdiff_usercomment     JD255
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.415
_reflns_odcompleteness_completeness 99.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Restrained distances
 H4A-O4
 0.88 with sigma of 0.02
 O4-H4B
 0.88 with sigma of 0.02
2.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4), C5(H5), C12(H12), C13(H13), C14(H14)
2.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;
_shelx_res_checksum              95148
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.682
_oxdiff_exptl_absorpt_empirical_full_min 0.708