Robust and Porous β-Diketiminate-Functionalized Metal-Organic Frameworks for Earth-Abundant-Metal-Catalyzed C-H Amination and Hydrogenation.
Thacker, Nathan C.; Lin, Zekai; Zhang, Teng; Gilhula, James C.; Abney, Carter W.; Lin, Wenbin; Journal of the American Chemical Society 138 (2016) 3501–3509; doi:10.1021/jacs.5b13394

data_4130053
_publ_section_title
;
 Robust and Porous \b-Diketiminate-Functionalized Metal-Organic Frameworks
 for Earth-Abundant-Metal-Catalyzed C-H Amination and Hydrogenation.
;
_journal_issue                   10
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3501
_journal_page_last               3509
_journal_paper_doi               10.1021/jacs.5b13394
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C17 H18 Cl2 Co N2'
_chemical_formula_sum            'C17 H18 Cl2 Co N2'
_chemical_formula_weight         380.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-09-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.21 svn.r3230 for OlexSys, GUI svn.r5100)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.305(2)
_cell_length_b                   22.491(4)
_cell_length_c                   7.4571(15)
_cell_measurement_reflns_used    2662
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      15.1075
_cell_measurement_theta_min      2.3577
_cell_volume                     1728.3(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.774
_diffrn_measured_fraction_theta_max 0.754
_diffrn_measurement_device_type  'synchrotron, beamline 15-ID, APEX2 detector'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           'synchrotron radiation'
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0860
_diffrn_reflns_av_unetI/netI     0.1002
_diffrn_reflns_Laue_measured_fraction_full 0.774
_diffrn_reflns_Laue_measured_fraction_max 0.754
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3785
_diffrn_reflns_point_group_measured_fraction_full 0.561
_diffrn_reflns_point_group_measured_fraction_max 0.528
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         15.141
_diffrn_reflns_theta_min         1.559
_exptl_absorpt_coefficient_mu    0.257
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       needle
_exptl_crystal_F_000             780
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 333 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         1926
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0806
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0472P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1135
_reflns_Friedel_coverage         0.298
_reflns_Friedel_fraction_full    0.309
_reflns_Friedel_fraction_max     0.263
_reflns_number_gt                1468
_reflns_number_total             1926
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b13394_si_002.cif
_cod_data_source_block           conacnac2_solve_a
_cod_database_code               4130053
_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
2. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 C12, C13, C14, C15, C16, C17
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C6, C7, C8, C9, C10, C11
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              53544
_shelx_hkl_checksum              13083
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'