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_7708002
_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 H33 Cl Cu N2 O2'
_chemical_formula_sum            'C24 H33 Cl Cu N2 O2'
_chemical_formula_weight         480.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_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                   11.2264(2)
_cell_length_b                   11.5091(3)
_cell_length_c                   35.7717(8)
_cell_measurement_reflns_used    14699
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.1550
_cell_measurement_theta_min      2.5870
_cell_volume                     4621.91(18)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (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    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.997
_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   -110.00  33.00   0.50   60.00    --  -20.40 -43.00-166.00  286
  2  \w    -58.00  69.00   0.50   60.00    --  -20.40  60.00-180.00  254
  3  \w   -110.00  17.00   0.50   60.00    --  -20.40 -60.00  30.00  254
  4  \w    -58.00  -8.00   0.50   60.00    --  -20.40  60.00 -30.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type
;
Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HyPix 6000 detector
;
_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      0.0020229000
_diffrn_orient_matrix_UB_12      -0.0001439000
_diffrn_orient_matrix_UB_13      -0.0198244000
_diffrn_orient_matrix_UB_21      0.0533103000
_diffrn_orient_matrix_UB_22      -0.0330424000
_diffrn_orient_matrix_UB_23      0.0005402000
_diffrn_orient_matrix_UB_31      -0.0338225000
_diffrn_orient_matrix_UB_32      -0.0520196000
_diffrn_orient_matrix_UB_33      -0.0002989000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            50406
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.000
_diffrn_reflns_theta_min         2.142
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    1.083
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       '(cut) plate'
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         7359
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0272P)^2^+4.2859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5755
_reflns_number_total             7359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01950c2.cif
_cod_data_source_block           2019ncsx0501z
_cod_depositor_comments
'Adding full bibliography for 7708002--7708009.cif.'
_cod_database_code               7708002
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'C22 H31 Cl Cu N2 O2 '
_chemical_oxdiff_usercomment     JD337
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.899
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.93
_olex2_refinement_description
;
1. Restrained distances
 O2-C20 \\sim O3-C24
 with sigma of 0.02
2. Others
 Sof(O3)=Sof(H3)=Sof(H20)=1-FVAR(1)
 Sof(O2)=Sof(H2)=Sof(H24)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 N2(H2A)
3.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C15(H15), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
3.e Idealised tetrahedral OH refined with riding coordinates:
 O3(H3)
3.f Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              65844
_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 2.817
_oxdiff_exptl_absorpt_empirical_full_min 0.323