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_7708005
_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
'2(C21 H26 Cu N2 O3), C42 H54 Cu2 N4 O7, 2(C H4 O), 2(O), 4(H2 O)'
_chemical_formula_sum            'C86 H122 Cu4 N8 O21'
_chemical_formula_weight         1858.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-05-17
_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                 96.7456(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.19436(19)
_cell_length_b                   14.08347(11)
_cell_length_c                   25.8393(3)
_cell_measurement_reflns_used    26034
_cell_measurement_temperature    173
_cell_measurement_theta_max      67.7720
_cell_measurement_theta_min      3.6830
_cell_volume                     8743.55(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (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 2014/1 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_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  79.00   1.00    5.00    --    0.00  60.00 120.00  168
  2  \w    -57.00   0.00   1.00   15.00    --  -89.00  60.00-167.78   57
  3  \w   -171.00   0.00   1.00   15.00    --  -89.00  60.00-139.31  171
  4  \w    -69.00  -1.00   1.00   15.00    --  -89.00  58.00-176.87   68
  5  \w   -157.00-113.00   1.00   15.00    --  -89.00  58.00  49.63   44
  6  \w    -89.00 -58.00   1.00   15.00    --  -89.00  58.00  49.63   31
  7  \w    -40.00   0.00   1.00   15.00    --  -89.00  58.00  49.63   40
  8  \w   -177.00-108.00   1.00   15.00    --  -89.00  58.00 128.37   69
  9  \w    -75.00  -1.00   1.00   15.00    --  -89.00  58.00 128.37   74
 10  \w    -29.00   0.00   1.00   15.00    --  -89.00  57.00-116.05   29
 11  \w   -175.00-143.00   1.00   15.00    --  -89.00  10.00-180.00   32
 12  \w    -98.00 -71.00   1.00   15.00    --  -89.00  10.00-180.00   27
 13  \w    -47.00 -20.00   1.00   15.00    --  -89.00  10.00-180.00   27
 14  \w   -178.00 -20.00   1.00   15.00    --  -89.00  40.00 150.00  158
 15  \w   -150.00-118.00   1.00   15.00    --  -89.00  58.00-176.87   32
 16  \w    -73.00   0.00   1.00   15.00    --  -89.00  58.00 -44.31   73
 17  \w   -166.00-141.00   1.00   15.00    --  -89.00  60.00 103.63   25
 18  \w   -112.00 -85.00   1.00   15.00    --  -89.00  60.00 103.63   27
 19  \w    -73.00  -2.00   1.00   15.00    --  -89.00  60.00 103.63   71
 20  \w   -125.00 -39.00   1.00   15.00    --  -89.00  57.00-116.05   86
 21  \w   -119.00 -94.00   1.00   15.00    --  -89.00  60.00-167.78   25
 22  \w   -130.00-105.00   1.00   15.00    --  -89.00  59.00-152.26   25
 23  \w    -25.00   0.00   1.00   15.00    --  -89.00  59.00-152.26   25
 24  \w    -27.00  -2.00   1.00   15.00    --  -89.00  59.00-132.37   25
 25  \w   -107.00 -82.00   1.00   15.00    --  -89.00  10.00  30.00   25
 26  \w    -29.00  -2.00   1.00   15.00    --  -89.00  10.00  30.00   27
 27  \w   -155.00-130.00   1.00   15.00    --  -89.00  60.00 -58.19   25
 28  \w   -163.00-136.00   1.00   15.00    --  -89.00  60.00 164.50   27
 29  \w    -25.00   0.00   1.00   15.00    --  -89.00  60.00-160.93   25
 30  \w    -26.00  -1.00   1.00   15.00    --  -89.00  60.00-124.08   25
 31  \w    -40.00   0.00   1.00   15.00    --  -89.00  58.00-122.75   40
;
_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      0.0176689000
_diffrn_orient_matrix_UB_12      -0.0380436000
_diffrn_orient_matrix_UB_13      -0.0514910000
_diffrn_orient_matrix_UB_21      -0.0201144000
_diffrn_orient_matrix_UB_22      -0.0999684000
_diffrn_orient_matrix_UB_23      0.0131696000
_diffrn_orient_matrix_UB_31      -0.0582672000
_diffrn_orient_matrix_UB_32      0.0228839000
_diffrn_orient_matrix_UB_33      -0.0279141000
_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  0.0283
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            54226
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.009
_diffrn_reflns_theta_min         4.862
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.714
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63556
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             3912
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.674
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         7901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0697
_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^)+(0.0924P)^2^+28.7852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1919
_refine_ls_wR_factor_ref         0.1934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7581
_reflns_number_total             7901
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01950c2.cif
_cod_data_source_block           jd511a
_cod_depositor_comments
'Adding full bibliography for 7708002--7708009.cif.'
_cod_original_cell_volume        8743.56(13)
_cod_database_code               7708005
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'C122 H122 N122 O122 Cu122 '
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.919
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Sof: O8(0.5) H8A(0.5) H8B(0.5)
2.a Free rotating group:
 O9(H9C,H9D), O12(H12C,H12D)
2.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), C8(H8), C13(H13), N3(H3), N4(H4), C29(H29), C34(H34)
2.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C14(H14A,H14B), C28(H28A,H28B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B),
  C33(H33A,H33B), C35(H35A,H35B), O8(H8A,H8B)
2.d Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3A), C4(H4A), C5(H5), C16(H16), C17(H17), C18(H18), C23(H23),
 C24(H24), C25(H25), C26(H26), C37(H37), C38(H38), C39(H39)
2.e Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C42(H42A,H42B,H42C), C01N(H01A,H01B,H01C)
2.f Idealised tetrahedral OH refined as rotating group:
 O10(H10)
;
_shelx_res_checksum              567
_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 1.635
_oxdiff_exptl_absorpt_empirical_full_min 0.663