A New Class of Metal-Cyclam based Zirconium Metal-Organic Frameworks for CO2 Adsorption and Chemical Fixation.
Zhu, Jie; Usov, Pavel M.; Xu, Wenqian; Celis-Salazar, Paula J; Lin, Shaoyang; Kessinger, Matthew C.; Landaverde-Alvarado, Carlos; Cai, Meng; May, Ann M.; Slebodnick, Carla; Zhu, Dunru; Senanayake, Sanjaya D.; Morris, Amanda J.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b10643

data_4127027
_publ_section_title
;
 A New Class of Metal-Cyclam based Zirconium Metal-Organic Frameworks for
 CO2 Adsorption and Chemical Fixation.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b10643
_journal_year                    2017
_chemical_formula_moiety
'C6 H12 Cl Cu0.5 N2 O6, C6 H12 Cu0.5 N2 O2, Cl O4'
_chemical_formula_sum            'C12 H24 Cl2 Cu N4 O12'
_chemical_formula_weight         550.79
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                90.048(4)
_cell_angle_beta                 104.471(5)
_cell_angle_gamma                95.762(4)
_cell_formula_units_Z            2
_cell_length_a                   8.5135(5)
_cell_length_b                   9.7381(4)
_cell_length_c                   13.3092(7)
_cell_measurement_reflns_used    3606
_cell_measurement_temperature    101.55(10)
_cell_measurement_theta_max      31.5210
_cell_measurement_theta_min      3.8210
_cell_volume                     1062.61(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_environment      N~2~
_diffrn_ambient_temperature      101.55(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0061
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_details
;
  1 omega  -52.00   37.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.6878   57.0000  -60.0000 89

  2 omega  -69.00   36.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.6878   90.0000 -175.0000 105

  3 omega  -81.00   -2.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.6878  -77.0000    0.0000 79

  4 omega -100.00  -57.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.6878  -57.0000  150.0000 43

  5 omega -102.00  -15.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.6878  -77.0000   90.0000 87

  6 omega -111.00  -74.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.6878  178.0000 -150.0000 37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0576099000
_diffrn_orient_matrix_UB_12      0.0058169000
_diffrn_orient_matrix_UB_13      -0.0305423000
_diffrn_orient_matrix_UB_21      0.0564664000
_diffrn_orient_matrix_UB_22      -0.0308917000
_diffrn_orient_matrix_UB_23      0.0396976000
_diffrn_orient_matrix_UB_31      -0.0312576000
_diffrn_orient_matrix_UB_32      -0.0661444000
_diffrn_orient_matrix_UB_33      -0.0228663000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11232
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.250
_diffrn_reflns_theta_min         3.752
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.347
_exptl_absorpt_correction_T_max  0.820
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent purple'
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_description       prism
_exptl_crystal_F_000             566
_exptl_crystal_size_max          0.3601
_exptl_crystal_size_mid          0.3204
_exptl_crystal_size_min          0.1954
_refine_diff_density_max         1.573
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         6900
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0384P)^2^+1.1926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1221
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5212
_reflns_number_total             6900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10643_si_005.cif
_cod_data_source_block           xpc115abs
_cod_database_code               4127027
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Cu N4 O8 Cl C12 H22'
_chemical_oxdiff_usercomment     'JIE ZHU CuL(ClO4)2'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N3(H3A), N4(H4), C8(H8), N1(H1A), N2(H2), C2(H2A)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C3(H3B,H3C),
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
;
_shelx_res_checksum              57312
_shelx_hkl_checksum              34701
_olex2_submission_special_instructions 'No special instructions were received'