Conformational studies of ligand-template assemblies and the consequences for encapsulation of rhodium complexes and hydroformylation catalysis
Jacobs, Ivo; van Duin, Adri C. T.; Kleij, Arjan W.; Kuil, Mark; Tooke, Duncan M.; Spek, Anthony L.; Reek, Joost N. H.; Catalysis Science & Technology 3 (2013) 1955–; doi:10.1039/c3cy20665c

data_1556383
_publ_section_title
;
 Conformational studies of ligand-template assemblies and the consequences
 for encapsulation of rhodium complexes and hydroformylation catalysis
;
_journal_issue                   8
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              1955
_journal_paper_doi               10.1039/c3cy20665c
_journal_volume                  3
_journal_year                    2013
_chemical_formula_moiety         'C99 H102 N9 O6 P Zn3'
_chemical_formula_sum            'C99 H102 N9 O6 P Zn3'
_chemical_formula_weight         1741.04
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            8
_cell_length_a                   20.8644(4)
_cell_length_b                   20.8644(4)
_cell_length_c                   52.9489(13)
_cell_measurement_reflns_used    237
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      13.675
_cell_measurement_theta_min      3.206
_cell_volume                     19961.8(7)
_computing_cell_refinement       DIRAX
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        'EvalCCD and SADABS'
_computing_molecular_graphics    PLATON
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    DIRDIF
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0974
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            204945
_diffrn_reflns_theta_full        22.48
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.9
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7296
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.14
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.387
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         8702
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+15.8981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1185
_reflns_number_gt                7387
_reflns_number_total             8702
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3cy20665c.txt
_cod_data_source_block           s3343a
_cod_database_code               1556383