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_4127028
_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 Cu N4 O4'
_chemical_formula_sum            'C12 H24 Cl2 Cu N4 O4'
_chemical_formula_weight         422.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-03-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.913(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.7984(4)
_cell_length_b                   9.7309(5)
_cell_length_c                   12.9543(7)
_cell_measurement_reflns_used    3360
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.8840
_cell_measurement_theta_min      3.7790
_cell_volume                     854.99(8)
_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 8.0061
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_details
;
  1 omega  -99.00   23.00   1.0000   41.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -19.0000 -120.0000 122

  2 omega -100.00   -4.00   1.0000   41.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -65.0000   55.0000 96

  3 omega  -54.00   38.00   1.0000   41.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   65.0000 -168.0000 92

  4 omega -109.00  -57.00   1.0000   41.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000  120.0000 52

  5 omega -101.00  -48.00   1.0000   41.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315 -178.0000 -120.0000 53

  6 omega  -62.00  -32.00   1.0000   41.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315   77.0000  -30.0000 30

  7 omega  -25.00    7.00   1.0000   41.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.5315  -83.0000    0.9133 32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0038310000
_diffrn_orient_matrix_UB_12      -0.0662897000
_diffrn_orient_matrix_UB_13      -0.0225981000
_diffrn_orient_matrix_UB_21      -0.0685369000
_diffrn_orient_matrix_UB_22      -0.0244083000
_diffrn_orient_matrix_UB_23      0.0346573000
_diffrn_orient_matrix_UB_31      -0.0788744000
_diffrn_orient_matrix_UB_32      0.0178839000
_diffrn_orient_matrix_UB_33      -0.0360902000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9225
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        30.520
_diffrn_reflns_theta_max         32.346
_diffrn_reflns_theta_min         3.662
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.613
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.771
_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    1.642
_exptl_crystal_description       block
_exptl_crystal_F_000             438
_exptl_crystal_size_max          0.2009
_exptl_crystal_size_mid          0.1038
_exptl_crystal_size_min          0.0614
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0257P)^2^+0.5131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0803
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2307
_reflns_number_total             2782
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10643_si_003.cif
_cod_data_source_block           xpc68abs
_cod_original_cell_volume        854.98(8)
_cod_database_code               4127028
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'Cu C12 N4 O4 Zr H22'
_chemical_oxdiff_usercomment     'XPC68 Jie Zhu JZ-2-P-114-1'
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1A(0.016) H2(0.014) H1B(0.02) H1C(0.02) H2A(0.019) H2B(0.019)
 H3A(0.02) H3B(0.02) H4A(0.016) H4B(0.016) H5(0.019)
 Fixed X: Cu1(0.5) H1A(0.3296) H2(0.8198) H1B(0.5746) H1C(0.4115) H2A(0.5829)
 H2B(0.741) H3A(0.76) H3B(0.5271) H4A(0.5427) H4B(0.7742) H5(0.8406)
 Fixed Y: Cu1(0.5) H1A(0.4435) H2(0.5979) H1B(0.2152) H1C(0.2245) H2A(0.4387)
 H2B(0.4054) H3A(0.6423) H3B(0.6594) H4A(0.8147) H4B(0.8278) H5(0.7613)
 Fixed Z: Cu1(0.5) H1A(0.3274) H2(0.4502) H1B(0.3798) H1C(0.285) H2A(0.2235)
 H2B(0.318) H3A(0.281) H3B(0.2912) H4A(0.4334) H4B(0.4197) H5(0.5964)
;
_shelx_res_checksum              54939
_shelx_hkl_checksum              90015
_olex2_submission_original_sample_id XPC68
_olex2_submission_special_instructions 'No special instructions were received'