Reinforced cyclam derivatives functionalized on the bridging unit
Sok, Nicolas; Baglin, Isabelle; Rousselin, Yoann; Boschetti, Frederic; Bernhard, Claire; Goze, Christine; Denat, Franck; New J. Chem. 40 (2016) 5829–; doi:10.1039/C5NJ03488D

data_7055445
_publ_section_title
;
 Reinforced cyclam derivatives functionalized on the bridging unit
;
_journal_issue                   7
_journal_name_full               'New J. Chem.'
_journal_page_first              5829
_journal_paper_doi               10.1039/C5NJ03488D
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C15 H27 N5'
_chemical_formula_sum            'C15 H27 N5'
_chemical_formula_weight         277.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-18
_audit_creation_method
;
Olex2 1.2
(compiled Sep 16 2015 11:44:03 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-11-26 deposited with the CCDC.
2016-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                78.653(2)
_cell_angle_beta                 80.2470(10)
_cell_angle_gamma                73.002(2)
_cell_formula_units_Z            4
_cell_length_a                   9.8695(3)
_cell_length_b                   12.1158(3)
_cell_length_c                   14.4185(5)
_cell_measurement_reflns_used    6734
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     1605.02(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      115
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean 9
_diffrn_detector_type            CCD
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f and \w scans''
_diffrn_orient_matrix_type       'Nonius Collect from scalepack cell'
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13714
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.506
_diffrn_reflns_theta_min         1.451
_diffrn_source                   'X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         7301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0165P)^2^+1.2470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1153
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5760
_reflns_number_total             7301
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {46137393-b90a-47c3-8acd-9511e03bacc4}
_cod_data_source_file            c5nj03488d2.cif
_cod_data_source_block           compound_4
_cod_depositor_comments
'Adding full bibliography for 7055444--7055449.cif.'
_cod_database_code               7055445
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.988
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB), C2A(H2AA,H2AB), C2B(H2BA,H2BB), C3A(H3AA,
 H3AB), C3B(H3BA,H3BB), C4A(H4AA,H4AB), C4B(H4BA,H4BB), C5A(H5AA,H5AB),
 C5B(H5BA,H5BB), C6A(H6AA,H6AB), C6B(H6BA,H6BB), C7A(H7AA,H7AB), C7B(H7BA,H7BB),
  C8A(H8AA,H8AB), C8B(H8BA,H8BB), C9A(H9AA,H9AB), C9B(H9BA,H9BB), C10A(H10A,
 H10B), C10B(H10C,H10D)
2.b Aromatic/amide H refined with riding coordinates:
 C11A(H11A), C11B(H11B)
2.c Idealised Me refined as rotating group:
 C21A(H21A,H21B,H21C), C21B(H21D,H21E,H21F), C41A(H41A,H41B,H41C), C41B(H41D,
 H41E,H41F)
;
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a glass fibre with grease'
_olex2_submission_special_instructions 'No special instructions were received'