Naphthalene-based linkers for metal phosphonates: synthesis, structure, and interesting conformational flexibility influence on final lanthanum hybrids
Białek, Michał J.; Janczak, Jan; Zoń, Jerzy; CrystEngComm 15 (2013) 390–; doi:10.1039/c2ce26268a

data_7210630
_publ_section_title
;
 Naphthalene-based linkers for metal phosphonates: synthesis, structure,
 and interesting conformational flexibility influence on final lanthanum
 hybrids
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              390
_journal_paper_doi               10.1039/c2ce26268a
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C11 H12 O6 P2, 2(H2 O)'
_chemical_formula_sum            'C11 H16 O8 P2'
_chemical_formula_weight         338.18
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 91.50(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.492(3)
_cell_length_b                   8.066(1)
_cell_length_c                   15.534(2)
_cell_measurement_reflns_used    1982
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.65
_cell_measurement_theta_min      2.98
_cell_volume                     2817.2(6)
_computing_cell_refinement
;
Oxford Diffraction Poland (2006). CrysAlis Red, Version 171.32.6
;
_computing_data_collection
;
Oxford Diffraction Poland (2006). CrysAlis CCD, Version 171.32.6
;
_computing_data_reduction
;
Oxford Diffraction Poland (2006). CrysAlis Red, Version 171.32.6
;
_computing_molecular_graphics
;
Brandenburg & Putz (2006). Diamond 3.0. Crystal and Molecular
Structure Visualisation, University of Bonn, Germany
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'KUMA KM-4 with area CCD detector'
_diffrn_measurement_method       \w-scan
_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  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18874
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         29.29
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    0.345
_exptl_absorpt_correction_T_max  0.9321
_exptl_absorpt_correction_T_min  0.8923
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Oxford Diffraction Poland (2006). CrysAlis Red, Version 171.32.6
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_meas      1.59
_exptl_crystal_density_method    floatation
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0026(2)
_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   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3610
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0275
_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^)+(0.0415P)^2^+1.5063P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                2879
_reflns_number_total             3610
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2ce26268a.txt
_cod_data_source_block           NDP(1,4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7210630