Construction of the First Rhodium(I) Cyclic Pentameric Structure [Rh(CO)Cl{(μ-N(t)BuP)2(C≡CPh)2}]5 Using (Phenylethynyl)cyclodiphosphazanes.
Siddiqui, Mujahuddin M.; Mague, Joel T.; Balakrishna, Maravanji S.; Inorganic chemistry 54 (2015) 1200–1202; doi:10.1021/ic5028042

data_4342183
_publ_section_title
;
 Construction of the First Rhodium(I) Cyclic Pentameric Structure
 [Rh(CO)Cl{(\m-N(t)BuP)2(C\\tb CPh)2}]5 Using
 (Phenylethynyl)cyclodiphosphazanes.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1200
_journal_page_last               1202
_journal_paper_doi               10.1021/ic5028042
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C24 H28 N2 P2'
_chemical_formula_sum            'C24 H28 N2 P2'
_chemical_formula_weight         406.42
_chemical_name_systematic
; 
 1,3-Di-tert-butyl-2,4-bis(phenylethynyl)-[1,3,2,4]
diazadiphosphetidine 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 115.1720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6716(11)
_cell_length_b                   10.4009(7)
_cell_length_c                   15.5875(10)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.11
_cell_measurement_theta_min      2.43
_cell_volume                     2299.5(3)
_computing_cell_refinement       'SAINT (Bruker-AXS 2009a)'
_computing_data_collection       'APEX2 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT (Bruker-AXS 2009a)'
_computing_molecular_graphics    'SHELXTL(Bruker-AXS 2008)'
_computing_publication_material  'SHELXTL(Bruker-AXS 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40439
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        28.750
_diffrn_reflns_theta_max         29.161
_diffrn_reflns_theta_min         2.428
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008a)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slab
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.172
_exptl_transmission_factor_max   0.966
_exptl_transmission_factor_min   0.906
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.0036(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         6079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+0.8515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.1019
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5120
_reflns_number_total             6079
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5028042_si_002.cif
_cod_data_source_block           MSB459_1m
_cod_depositor_comments
'Adding full bibliography for 4342183--4342185.cif.'
_cod_database_code               4342183
_shelx_estimated_absorpt_t_min   0.939
_shelx_estimated_absorpt_t_max   0.966
_shelxl_version_number           2014/6
_shelx_res_checksum              49728
_shelx_hkl_checksum              48252