Modulation of the CO2 fixation in dinickel azacryptands.
Möller, F; Castañeda-Losada, L; Junqueira, J. R. C.; Miller, R. G.; Reback, M. L.; Mallick, B.; van Gastel, M.; Apfel, U.-P.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5680–5688; doi:10.1039/c6dt04527h

data_7041954
_publ_section_title
;
 Modulation of the CO2 fixation in dinickel azacryptands.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5680
_journal_page_last               5688
_journal_paper_doi               10.1039/c6dt04527h
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C36 H39 F3 N8'
_chemical_formula_sum            'C36 H39 F3 N8'
_chemical_formula_weight         640.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-01-10 deposited with the CCDC.
2017-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.98(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.888(3)
_cell_length_b                   13.4639(18)
_cell_length_c                   16.442(3)
_cell_measurement_reflns_used    6746
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      36.5984
_cell_measurement_theta_min      2.9056
_cell_volume                     3427.3(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 8.4171
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_av_unetI/netI     0.2518
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17944
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.220
_diffrn_reflns_theta_min         2.527
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.9937
_exptl_absorpt_correction_T_min  0.9682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       prism
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 621 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.7(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.782
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         7944
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.782
_refine_ls_R_factor_all          0.2070
_refine_ls_R_factor_gt           0.0793
_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^)+(0.1025P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2261
_refine_ls_wR_factor_ref         0.2570
_reflns_Friedel_coverage         0.939
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.926
_reflns_number_gt                11896
_reflns_number_total             17944
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {0f572e16-c84f-4356-bae3-ad4ddf93468d}
_cod_data_source_file            c6dt04527h2.cif
_cod_data_source_block           LIF_lc-27a
_cod_depositor_comments
'Adding full bibliography for 7041952--7041960.cif.'
_cod_database_code               7041954
_cell_oxdiff_measurement_reflns_used 6757
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4571 0.22245 0.17525 0.09637 0.04883
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B),
  C35(H35A,H35B), C36(H36A,H36B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C9(H9), C10(H10), C15(H15), C17(H17), C19(H19),
 C24(H24), C21(H21), C27(H27), C29(H29), C31(H31), C33(H33), C34(H34)
3.c Fitted hexagon refined as free rotating group:
 C4(C5,C6,C7,C8,C9), C16(C17,C18,C19,C20,C24), C28(C29,C30,C31,C32,C33)
;
_shelx_res_checksum              84242
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'