Convergent Synthesis of a Metal‒Organic Framework Supported Olefin Metathesis Catalyst
Yuan, Jian; Fracaroli, Alejandro M.; Klemperer, Walter G.; Organometallics 35 (2016) 2149–; doi:10.1021/acs.organomet.6b00365

data_4088731
_publ_section_title
;
 Convergent Synthesis of a Metal--Organic Framework Supported Olefin
 Metathesis Catalyst
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2149
_journal_paper_doi               10.1021/acs.organomet.6b00365
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C38 H42 N2 O4 Ru'
_chemical_formula_sum            'C38 H42 N2 O4 Ru'
_chemical_formula_weight         691.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                95.940(2)
_cell_angle_beta                 103.7630(10)
_cell_angle_gamma                113.2560(10)
_cell_formula_units_Z            2
_cell_length_a                   10.1410(3)
_cell_length_b                   10.5310(3)
_cell_length_c                   18.1578(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1687.57(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.955
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24745
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.320
_diffrn_reflns_theta_min         2.569
_exptl_absorpt_coefficient_mu    4.089
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1161 before and 0.0667 after correction. The Ratio of minimum to maximum transmission is 0.6235. The \l/2 correction factor is 0.0015.'
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       prism
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         5920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0473P)^2^+0.9829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4876
_reflns_number_total             5920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00365_si_002.cif
_cod_data_source_block           ru-cat
_cod_original_cell_volume        1687.57(8)
_cod_database_code               4088731
_shelxl_version_number           2014-3
_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.a Ternary CH refined with riding coordinates:
 C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C64(H64A,H64B)
2.c Aromatic/amide H refined with riding coordinates:
 C28(H28), C29(H29), C36(H36), C39(H39), C47(H47), C56(H56), C63(H63),
 C65(H65), C72(H72), C76(H76), C78(H78), C81(H81), C82(H82)
2.d Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C1C(H1CA,H1CB,H1CC), C1E(H1EA,H1EB,H1EC), C2(H2A,H2B,
 H2C), C3(H3A,H3B,H3C), C7(H7A,H7B,H7C), C34(H34A,H34B,H34C), C90(H90A,H90B,
 H90C)
;
_olex2_submission_special_instructions 'No special instructions were received'