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_4127030
_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 N4 Ni O4, 2(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C12 H28 Cl2 N4 Ni O14'
_chemical_formula_weight         581.99
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 103.592(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.5347(5)
_cell_length_b                   15.2793(11)
_cell_length_c                   8.7620(7)
_cell_measurement_reflns_used    3581
_cell_measurement_temperature    250.00(14)
_cell_measurement_theta_max      74.2440
_cell_measurement_theta_min      5.1900
_cell_volume                     1110.60(14)
_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      250.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1587
_diffrn_detector_type            Onyx
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega -107.00  -80.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6919  -99.0000 -120.0000 27

  2 omega -110.00  -21.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6919  -57.0000  120.0000 89

  3 omega  -96.00   -6.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6919  125.0000    0.0000 90

  4 omega  -69.00   27.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6919   57.0000  -90.0000 96

  5 omega   81.00  117.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6919  125.0000   90.0000 36

  6 omega   31.00   96.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000 -111.0000  150.0000 65

  7 omega   34.00   65.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -45.0000  150.0000 31

  8 omega   36.00   64.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000 -111.0000  -30.0000 28

  9 omega   29.00   56.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -77.0000 -120.0000 27

 10 omega  125.00  164.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000   15.0000  -90.0000 39

 11 omega   68.00   95.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -77.0000 -120.0000 27

 12 omega  111.00  140.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -77.0000 -120.0000 29

 13 omega   55.00  124.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -77.0000   60.0000 69

 14 omega   80.00  107.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000   61.0000  120.0000 27

 15 omega   32.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000   30.0000 37

 16 omega   34.00   59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -45.0000 -120.0000 25

 17 omega   27.00   99.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000 -111.0000   60.0000 72

 18 omega   61.00   88.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000   15.0000  -90.0000 27

 19 omega   46.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000 -111.0000 -120.0000 59

 20 omega   36.00   76.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -61.0000  150.0000 40

 21 omega  101.00  133.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -61.0000  150.0000 32

 22 omega   31.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -15.0000  150.0000 39

 23 omega   74.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -15.0000  150.0000 29

 24 omega  109.00  155.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -15.0000  150.0000 46

 25 omega   27.00   78.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000 -111.0000   90.0000 51

 26 omega   81.00  115.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000 -111.0000   90.0000 34

 27 omega   66.00  101.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000   15.0000   30.0000 35

 28 omega   34.00   59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -61.0000 -150.0000 25

 29 omega   86.00  134.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -61.0000 -150.0000 48

 30 omega   57.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -94.0000  150.0000 40

 31 omega  124.00  151.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000   61.0000  120.0000 27

 32 omega   78.00  110.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000 -111.0000  -30.0000 32

 33 omega  148.00  178.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000   15.0000   30.0000 30

 34 omega   83.00  172.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000   61.0000  150.0000 89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0827492000
_diffrn_orient_matrix_UB_12      0.0182244000
_diffrn_orient_matrix_UB_13      0.1731667000
_diffrn_orient_matrix_UB_21      -0.0104603000
_diffrn_orient_matrix_UB_22      0.0990861000
_diffrn_orient_matrix_UB_23      -0.0332166000
_diffrn_orient_matrix_UB_31      -0.1659104000
_diffrn_orient_matrix_UB_32      0.0025908000
_diffrn_orient_matrix_UB_33      0.0408295000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10087
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        74.000
_diffrn_reflns_theta_max         75.089
_diffrn_reflns_theta_min         5.332
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.193
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.626
_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_density_diffrn    1.740
_exptl_crystal_description
;
;
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.2142
_exptl_crystal_size_mid          0.0997
_exptl_crystal_size_min          0.0385
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2266
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0637
_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^)+(0.0665P)^2^+1.6522P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1593
_refine_ls_wR_factor_ref         0.1650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2008
_reflns_number_total             2266
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10643_si_004.cif
_cod_data_source_block           xpc16_250abs
_cod_original_cell_volume        1110.59(14)
_cod_database_code               4127030
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C12 Ni N4 O12 Cl2 H20'
_chemical_oxdiff_usercomment
'Sample name JZ-1-p-104 Jie Zhu, Amanda Morris Lab'
_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 O(H) groups, All O(H,H) groups
2. Rigid body (RIGU) restrains
 Cl1, O5B, O5A, O4A, O4B, O7, O3A, O3B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(O3B)=Sof(O4B)=Sof(O5B)=1-FVAR(1)
 Sof(O3A)=Sof(O4A)=Sof(O5A)=FVAR(1)
4.a Free rotating group:
 O7(H7A,H7B)
4.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2A), C5(H5)
4.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2B,H2C), C3(H3A,H3B), C4(H4A,H4B)
;
_shelx_res_checksum              59227
_shelx_hkl_checksum              69401
_olex2_submission_special_instructions 'No special instructions were received'