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_4127026
_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         'C12 H24 Cl2 N4 Ni O4, 2(C3 H7 N O)'
_chemical_formula_sum            'C18 H38 Cl2 N6 Ni O6'
_chemical_formula_weight         564.15
_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     direct
_audit_creation_date             2017-03-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                71.886(4)
_cell_angle_beta                 86.219(4)
_cell_angle_gamma                73.762(5)
_cell_formula_units_Z            1
_cell_length_a                   6.5665(3)
_cell_length_b                   8.8382(5)
_cell_length_c                   11.8641(5)
_cell_measurement_reflns_used    4453
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.7420
_cell_measurement_theta_min      3.8810
_cell_volume                     628.15(6)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1587
_diffrn_detector_type            Onyx
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega  -31.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9419  -57.0000   90.0000 100

  2 omega  -37.00   76.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9419  -77.0000    0.0000 113

  3 omega  -31.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9419  -57.0000 -150.0000 100

  4 omega   27.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000 -111.0000 -120.0000 88

  5 omega   30.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000   60.0000 39

  6 omega   27.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000 -111.0000   60.0000 88

  7 omega   34.00  150.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  179.0000  -90.0000 116

  8 omega   33.00  136.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -61.0000 -150.0000 103

  9 omega   79.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  111.0000   90.0000 99

 10 omega   27.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000 -111.0000 -180.0000 88

 11 omega   33.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -45.0000  150.0000 44

 12 omega   27.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000 -111.0000  -30.0000 88

 13 omega   59.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000   15.0000  120.0000 119

 14 omega   30.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000  150.0000 39

 15 omega   34.00  150.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  179.0000 -120.0000 116

 16 omega   30.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000 -150.0000 39

 17 omega   77.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000   30.0000   30.0000 101

 18 omega   22.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -94.0000    0.0000 87

 19 omega   79.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  111.0000 -150.0000 99

 20 omega   33.00  136.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -61.0000   30.0000 103

 21 omega -115.00  -41.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.9419  -57.0000 -150.0000 74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1784060000
_diffrn_orient_matrix_UB_12      -0.0711770000
_diffrn_orient_matrix_UB_13      -0.0205947000
_diffrn_orient_matrix_UB_21      -0.1180579000
_diffrn_orient_matrix_UB_22      0.1712904000
_diffrn_orient_matrix_UB_23      -0.0825090000
_diffrn_orient_matrix_UB_31      0.1182181000
_diffrn_orient_matrix_UB_32      -0.0440584000
_diffrn_orient_matrix_UB_33      -0.1069748000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7818
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        74.260
_diffrn_reflns_theta_max         74.979
_diffrn_reflns_theta_min         3.921
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.462
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.747
_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 colourless'
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       needle
_exptl_crystal_F_000             298
_exptl_crystal_size_max          0.1568
_exptl_crystal_size_mid          0.1092
_exptl_crystal_size_min          0.0477
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0468P)^2^+0.2005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2195
_reflns_number_total             2563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10643_si_002.cif
_cod_data_source_block           xpc39abs
_cod_database_code               4127026
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C12 Ni3 N4 O4 H22'
_chemical_oxdiff_usercomment     'A. Morris Lab Jie Zhu JZ-P-120-8'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1A), N2(H2), C3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1B,H1C), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9)
2.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              473
_shelx_hkl_checksum              49152
_olex2_submission_original_sample_id 'XPPC 39'
_olex2_submission_special_instructions 'No special instructions were received'