Carbene insertion into N-H bonds with size-selectivity induced by a microporous ruthenium-porphyrin metal-organic framework.
Chen, Lianfen; Cui, Hao; Wang, Yanhu; Liang, Xiang; Zhang, Li; Su, Cheng-Yong; Dalton transactions (Cambridge, England : 2003) 47 (2018) 3940–3946; doi:10.1039/c8dt00434j

data_7045638
_publ_section_title
;
 Carbene insertion into N-H bonds with size-selectivity induced by a
 microporous ruthenium-porphyrin metal-organic framework.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3940
_journal_page_last               3946
_journal_paper_doi               10.1039/c8dt00434j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '0.25(C564 H288 Hf48 N48 O220 Ru12)'
_chemical_formula_sum            'C141 H72 Hf12 N12 O55 Ru3'
_chemical_formula_weight         5259.19
_chemical_name_systematic        Ru-PMOF-1(Hf)
_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_Hall           '-I 4 2 3'
_space_group_name_H-M_alt        'I m -3 m'
_symmetry_space_group_name_Hall  '-I 4 2 3'
_symmetry_space_group_name_H-M   'I m -3 m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-04
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_audit_update_record
;
2018-01-31 deposited with the CCDC.
2018-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   38.4253(3)
_cell_length_b                   38.4253(3)
_cell_length_c                   38.4253(3)
_cell_measurement_reflns_used    3632
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.6180
_cell_measurement_theta_min      3.6210
_cell_volume                     56735.1(8)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            17091
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        65.957
_diffrn_reflns_theta_max         65.957
_diffrn_reflns_theta_min         3.638
_exptl_absorpt_coefficient_mu    4.738
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.616
_exptl_crystal_description       block
_exptl_crystal_F_000             9752
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
;
_refine_diff_density_max         1.163
_refine_diff_density_min         -1.413
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         4555
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0890
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1264P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2288
_refine_ls_wR_factor_ref         0.2399
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2906
_reflns_number_total             4555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00434j2.cif
_cod_data_source_block           123
_cod_depositor_comments          'Adding full bibliography for 7045638.cif.'
_cod_original_cell_volume        56735.2(12)
_cod_database_code               7045638
_shelx_estimated_absorpt_t_max   0.518
_shelx_estimated_absorpt_t_min   0.483
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H11 of C11, H10 of C10, H7 of C7, H8 of C8
 At 1.5 times of:
  H1 of C1, H5 of C5
2. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O2(0.125) C1(0.5) H1(0.5) C3(0.5) C2(0.5) C6(0.5) C11(0.5)
 H11(0.5) C10(0.5) H10(0.5) C9(0.25) C8(0.5) H8(0.5) C7(0.5) H7(0.5) C4(0.5)
 C5(0.5) H5(0.5) O5(0.5) C13(0.125)
4.a Riding coordinates:
 C1(H1), C11(H11,C10), C11(H10,C9,C8), C11(H8,C7), C11(H7), C5(H5)
4.b Fitted hexagon refined as free rotating group:
 C6(C11,O4,O3,O1,C12)
;
_shelx_res_checksum              15470
_shelx_shelxl_version_number     2014/7