Metal-Organic Frameworks Stabilize Mono(phosphine)-Metal Complexes for Broad-Scope Catalytic Reactions.
Sawano, Takahiro; Lin, Zekai; Boures, Dean; An, Bing; Wang, Cheng; Lin, Wenbin; Journal of the American Chemical Society 138 (2016) 9783–9786; doi:10.1021/jacs.6b06239

data_4130736
_publ_section_title
;
 Metal-Organic Frameworks Stabilize Mono(phosphine)-Metal Complexes for
 Broad-Scope Catalytic Reactions.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9783
_journal_page_last               9786
_journal_paper_doi               10.1021/jacs.6b06239
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         '0.02(C154 Ir3.25 O36 P4 Zr6)'
_chemical_formula_sum            'C2.61 Ir0.07 O0.61 P0.07 Zr0.1'
_chemical_formula_weight         65.52
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_audit_creation_date             2016-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                117.806(4)
_cell_angle_beta                 111.824(4)
_cell_angle_gamma                90.022(5)
_cell_formula_units_Z            59
_cell_length_a                   19.783(7)
_cell_length_b                   21.510(7)
_cell_length_c                   23.023(8)
_cell_measurement_reflns_used    2636
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      9.51
_cell_measurement_theta_min      2.27
_cell_volume                     7862(5)
_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      100.0
_diffrn_measured_fraction_theta_full 0.052
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measurement_device_type
'synchrontron, beamline 15-ID, APEX2 detector'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.1494
_diffrn_reflns_av_unetI/netI     0.1423
_diffrn_reflns_Laue_measured_fraction_full 0.052
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44606
_diffrn_reflns_point_group_measured_fraction_full 0.052
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         9.856
_diffrn_reflns_theta_min         0.660
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_T_max  0.7434
_exptl_absorpt_correction_T_min  0.6403
_exptl_crystal_density_diffrn    0.816
_exptl_crystal_description       'yellow needle'
_exptl_crystal_F_000             1820
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         8229
_refine_ls_number_restraints     505
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.2091
_refine_ls_R_factor_gt           0.1346
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3304
_refine_ls_wR_factor_ref         0.3683
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3399
_reflns_number_total             8229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b06239_si_002.cif
_cod_data_source_block           p-1
_cod_original_formula_sum        'C2.61 Ir0.07 O0.61 P0.07 Zr0.10'
_cod_database_code               4130736
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(C) groups, All C(C,C) groups
2. Restrained distances
 C76-C3AA
 1.55 with sigma of 0.02
 O1-Ir4
 2.4 with sigma of 0.02
 C33-C118
 1.5 with sigma of 0.02
 C8AA-C9
 1.6 with sigma of 0.02
 C9-C11
 2.6 with sigma of 0.02
 C9-C19
 2.6 with sigma of 0.02
 C33-C118
 1.5 with sigma of 0.02
 C33-C7AA
 2.6 with sigma of 0.02
 C33-C195
 2.6 with sigma of 0.02
3. Restrained planarity
 C5CA, C7AA, C29, C33, C81, C118, C132, C133, C140, C148, C168, C195
 with sigma of 0.1
 C5CA, C7AA, C29, C33, C81, C118, C132, C133, C140, C148, C168, C195
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 O0AA, O1, O2, O2AA, O3AA, O4AA, O5, O6, O7, O9, O10, O11, O12, O13, O14, O15,
 O27, O52, Zr1, Zr2, Zr3, P6, P7, Ir4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Fitted hexagon refined as free rotating group:
 C2BA(C53,C61,C0BA,C6AA,C5AA), C2CA(C3BA,C7BA,C3CA,C12,C32), C6BA(C90,C70,C129,
 C111,C141), C8AA(C11,C7,C59,C9BA,C19), C22(C39,C47,C6CA,C155,C72), C26(C34,C21,
 C5BA,C9AA,C25), C33(C81,C148,C5CA,C29,C133), C41(C16,C1AA,C78,C4AA,C1CA),
 C60(C4BA,C18,C9,C0CA,C159), C80(C260,C99,C74,C85,C174), C118(C7AA,C140,C168,
 C132,C195)
;
_shelx_res_checksum              66687
_shelx_hkl_checksum              9197
_olex2_submission_special_instructions 'No special instructions were received'