Synthesis and conformational structure of hydrazo-bridged homo calix[2]pyridine[2]triazines
Liang, Dong-Dong; Wang, Mei-Xiang; Organic Chemistry Frontiers 4 (2017) 1425–; doi:10.1039/C7QO00221A

data_1553772
_publ_section_title
;
 Synthesis and conformational structure of hydrazo-bridged homo
 calix[2]pyridine[2]triazines
;
_journal_issue                   7
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              1425
_journal_paper_doi               10.1039/C7QO00221A
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         '0.17(C32 H60 Co2 N16 O8), 0.67(Cl O4)'
_chemical_formula_sum            'C5.33 H10 Cl0.67 Co0.33 N2.67 O4'
_chemical_formula_weight         218.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-02-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-03-20 deposited with the CCDC.
2017-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.734(4)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   11.9766(4)
_cell_length_b                   19.3355(5)
_cell_length_c                   12.7804(4)
_cell_measurement_reflns_used    4256
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      75.5370
_cell_measurement_theta_min      4.6440
_cell_volume                     2688.09(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.968
_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    -93.00  -8.00   1.00    1.71    --  -40.81 125.00-180.00   85
  2  \w   -113.00 -16.00   1.00    1.71    --  -40.81 -38.00-120.00   97
  3  \w      2.00  60.00   1.00    1.71    --   40.81 -99.00 150.00   58
  4  \w     49.00  76.00   1.00    1.71    --   40.81-125.00 -60.00   27
  5  \w    145.00 172.00   1.00   15.00    --  111.58  77.00-120.00   27
  6  \w    135.00 178.00   1.00   15.00    --  111.58 125.00-180.00   43
  7  \w     39.00 130.00   1.00   15.00    --  111.58 -45.00  90.00   91
  8  \w     65.00  98.00   1.00   15.00    --  111.58 -95.00 -60.00   33
  9  \w     30.00  57.00   1.00   15.00    --  111.58 -95.00 -60.00   27
 10  \w     98.00 167.00   1.00   15.00    --  111.58  45.00-120.00   69
 11  \w     60.00 129.00   1.00   15.00    --  111.58 -61.00-180.00   69
 12  \w     97.00 166.00   1.00   15.00    --  111.58  30.00 -30.00   69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0491445000
_diffrn_orient_matrix_UB_12      0.0424606000
_diffrn_orient_matrix_UB_13      -0.1122890000
_diffrn_orient_matrix_UB_21      -0.1282973000
_diffrn_orient_matrix_UB_22      -0.0323942000
_diffrn_orient_matrix_UB_23      -0.0351551000
_diffrn_orient_matrix_UB_31      -0.0349584000
_diffrn_orient_matrix_UB_32      0.0590856000
_diffrn_orient_matrix_UB_33      0.0613253000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10664
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.560
_diffrn_reflns_theta_min         4.064
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.495
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_description       plate
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.314
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0627
_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^)+(0.1050P)^2^+1.1930P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1679
_refine_ls_wR_factor_ref         0.1785
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4633
_reflns_number_total             5464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qo00221a2.cif
_cod_data_source_block           exp_874
_cod_original_cell_volume        2688.08(17)
_cod_database_code               1553772
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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, All O(H,H) groups
2.a Rotating group:
 O2(H2A,H2B), O3(H3A,H3B), O4(H4A,H4B)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2C,H2D,H2E), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C)
;
_olex2_date_sample_data_collection 2017-02-12
_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 1.698
_oxdiff_exptl_absorpt_empirical_full_min 0.677