Synthesis of Mono-, Di-, and Trinuclear Rhodium Diphosphine Complexes Containing Light-Harvesting Fluorene Backbones.
Matsusaka, Yuko; Shitaya, Shoji; Nomura, Kotohiro; Inagaki, Akiko; Inorganic chemistry 56 (2017) 1027–1030; doi:10.1021/acs.inorgchem.6b02423

data_4345396
_publ_section_title
;
 Synthesis of Mono-, Di-, and Trinuclear Rhodium Diphosphine Complexes
 Containing Light-Harvesting Fluorene Backbones.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1027
_journal_page_last               1030
_journal_paper_doi               10.1021/acs.inorgchem.6b02423
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C138 H84 B Cl2 F4 O9 P6 Rh3'
_chemical_formula_weight         2538.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.810(2)
_cell_angle_beta                 97.870(2)
_cell_angle_gamma                96.877(2)
_cell_formula_units_Z            2
_cell_length_a                   15.8385(3)
_cell_length_b                   18.5609(4)
_cell_length_c                   21.8751(5)
_cell_measurement_reflns_used    26806
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      32.62
_cell_measurement_theta_min      1.87
_cell_volume                     5975.2(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  CCD
_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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            62620
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.9424
_exptl_absorpt_correction_T_min  0.7953
_exptl_crystal_colour            prismatic
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       yellow
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.312
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1334
_refine_ls_number_reflns         27347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.163
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0787P)^2^+8.8320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1514
_reflns_number_gt                20369
_reflns_number_total             27347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            3Ph.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4345396