Powder Diffraction Study of a Coordination Polymer Comprised of Rigid Building Blocks: [Rh2(O2CCH3)4.μ2-Se2C5H8-Se,Se']∞
Evgeny V. Dikarev; Roman V. Shpanchenko; Kristian W. Andreini; Eric Block; Jin Jin; Marina A. Petrukhina; Inorganic Chemistry 43 (2004) 5558–5563; doi:10.1021/ic049497u

data_4311499
_publ_section_title
;
 Powder Diffraction Study of a Coordination Polymer Comprised of Rigid
 Building Blocks: [Rh2(O2CCH3)4.\m2-Se2C5H8-Se,Se']\\infty
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5558
_journal_page_last               5563
_journal_paper_doi               10.1021/ic049497u
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'Se (C H2)2 C (C H2)2 Se'
_chemical_formula_sum            'C5 H8 Se2'
_chemical_formula_weight         226.03
_chemical_melting_point          68(1)
_chemical_name_common            diselenadispiroheptane
_chemical_name_systematic
; 
 2,6-diselenaspiro[3.3]heptane 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.5500(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.9123(4)
_cell_length_b                   19.6400(13)
_cell_length_c                   5.8877(4)
_cell_measurement_reflns_used    4852
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.13
_cell_measurement_theta_min      3.64
_cell_volume                     648.15(8)
_computing_cell_refinement       'SMART, SAINT'
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXCIF-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '0.3 deg wide \w exposures'
_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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5094
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    11.283
_exptl_absorpt_correction_T_max  0.3446
_exptl_absorpt_correction_T_min  0.1329
_exptl_absorpt_correction_type   'multi-scan (SADABS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.316
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.839
_refine_diff_density_min         -1.281
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       0.055(3)
_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   1.075
_refine_ls_hydrogen_treatment    allref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1506
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0604P)^2^+0.1148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0839
_reflns_number_gt                1414
_reflns_number_total             1506
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049497usi20040410_064452.cif
_cod_data_source_block           Se(CH2)2C(CH2)2Se
_cod_database_code               4311499