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_4345397
_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            'C37 H28 P2'
_chemical_formula_weight         534.53
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.695(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.550(6)
_cell_length_b                   11.690(5)
_cell_length_c                   17.615(7)
_cell_measurement_reflns_used    7187
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.10
_cell_volume                     2732(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28240
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.185
_exptl_absorpt_correction_T_max  0.9817
_exptl_absorpt_correction_T_min  0.9466
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6227
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1356
_refine_ls_wR_factor_ref         0.1427
_reflns_number_gt                5499
_reflns_number_total             6227
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            LPh.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4345397