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_7708004
_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         '6(C21 H23 Cu F3 N2 O3), 5(C H4 O)'
_chemical_formula_sum            'C131 H158 Cu6 F18 N12 O23'
_chemical_formula_weight         2991.92
_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
_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                104.492(8)
_cell_angle_beta                 103.593(6)
_cell_angle_gamma                102.304(8)
_cell_formula_units_Z            1
_cell_length_a                   12.0183(9)
_cell_length_b                   14.9866(16)
_cell_length_c                   20.1854(14)
_cell_measurement_reflns_used    3074
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.0660
_cell_measurement_theta_min      4.2690
_cell_volume                     3275.5(5)
_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)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1030
_diffrn_reflns_av_unetI/netI     0.1332
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18274
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.520
_diffrn_reflns_theta_min         4.534
_exptl_absorpt_coefficient_mu    1.915
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61570
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       needle
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         12116
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1596
_refine_ls_R_factor_gt           0.0892
_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^)+(0.0662P)^2^+15.1640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2133
_refine_ls_wR_factor_ref         0.2543
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6867
_reflns_number_total             12116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01950c2.cif
_cod_data_source_block           jd447
_cod_depositor_comments
'Adding full bibliography for 7708002--7708009.cif.'
_cod_database_code               7708004
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.775
_olex2_refinement_description
;
1. Restrained distances
 O11-C94
 1.43 with sigma of 0.02
 C2-O12
 1.43 with sigma of 0.02
 O10-C91
 1.43 with sigma of 0.02
2. Others
 Fixed Sof: O12(0.5) H12A(0.5) C2(0.5) H2A(0.5) H2B(0.5) H2C(0.5)
3.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), C12(H12), C17(H17), N3(H3), N4(H4), C41(H41), C46(H46),
 N5(H5), N6(H6A), C70(H70), C75(H75)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,
 H16B), C19(H19A,H19B), C39(H39A,H39B), C42(H42A,H42B), C43(H43A,H43B),
 C44(H44A,H44B), C45(H45A,H45B), C48(H48A,H48B), C68(H68A,H68B), C71(H71A,H71B),
  C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C77(H77A,H77B)
3.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C22(H22), C23(H23), C24(H24), C25(H25), C34(H34),
 C36(H36), C37(H37), C51(H51), C52(H52), C53(H53), C54(H54), C63(H63), C65(H65),
  C66(H66), C80(H80), C81(H81), C82(H82), C83(H83)
3.d Idealised Me refined as rotating group:
 C91(H91A,H91B,H91C), C94(H94A,H94B,H94C), C2(H2A,H2B,H2C)
3.e Idealised tetrahedral OH refined as rotating group:
 O10(H10), O11(H11), O12(H12A)
;
_shelx_res_checksum              39882
_olex2_submission_special_instructions 'No special instructions were received'