Chiral two bladed ML2 metallamacrocycles: design, structures and solution behavior
Soudry, Hannah; Desmarets, Christophe; Gontard, Geoffrey; Edgington, Tiffany; Cooksy, Andrew L.; Amouri, Hani; Dalton Trans.  (2017) –; doi:10.1039/C7DT01151B

data_7043742
_publ_section_title
;
 Chiral two bladed ML2 metallamacrocycles: design, structures and solution
 behavior
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01151B
_journal_year                    2017
_chemical_formula_moiety         'C68 H68 Co N8 O4, 2(B F4), 2(C2 H3 N)'
_chemical_formula_sum            'C72 H74 B2 Co F8 N10 O4'
_chemical_formula_weight         1375.96
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-02-22 deposited with the CCDC.
2017-07-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.1730(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.9304(11)
_cell_length_b                   9.2813(2)
_cell_length_c                   21.8455(7)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    200(1)
_cell_measurement_theta_max      29.69
_cell_measurement_theta_min      2.45
_cell_volume                     6746.3(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SXGRAPH (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      200(1)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            59038
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.551
_diffrn_reflns_theta_min         1.921
_exptl_absorpt_coefficient_mu    0.334
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2868
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.200
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         10317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0741P)^2^+7.4120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1479
_reflns_number_gt                7515
_reflns_number_total             10317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01151b2.cif
_cod_data_source_block           Compound_1
_cod_database_code               7043742
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              843