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_7210632
_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         'C22 H35 La O19 P4, 2(H2 O)'
_chemical_formula_sum            'C22 H39 La O21 P4'
_chemical_formula_weight         902.32
_chemical_name_systematic
;
?
;
_space_group_IT_number           8
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2y'
_symmetry_space_group_name_H-M   'C 1 m 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                 96.740(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.2113(2)
_cell_length_b                   26.5836(5)
_cell_length_c                   6.85560(10)
_cell_measurement_reflns_used    862
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.40
_cell_measurement_theta_min      2.99
_cell_volume                     1667.13(5)
_computing_cell_refinement
;
Oxford Diffraction Poland (2006). CrysAlis Red, Version
171.32.6, Wroc\/law, Poland
;
_computing_data_collection
;
Oxford Diffraction Poland (2006). CrysAlis CCD, Version
171.32.6, Wroc\/law, Poland
;
_computing_data_reduction
;
Oxford Diffraction Poland (2006). CrysAlis Red, Version
171.32.6, Wroc\/law, Poland
;
_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 0.988
_diffrn_measured_fraction_theta_max 0.934
_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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11315
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         29.40
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    1.560
_exptl_absorpt_correction_T_max  0.8311
_exptl_absorpt_correction_T_min  0.5893
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Oxford Diffraction Poland (2006). CrysAlis Red, Version
171.32.6, Wroc\/law, Poland
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_density_meas      1.795
_exptl_crystal_density_method    floatation
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3506
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0173
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0413
_refine_ls_wR_factor_ref         0.0417
_reflns_number_gt                3464
_reflns_number_total             3506
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c2ce26268a.txt
_cod_data_source_block           La-NDP(1,4C)
_cod_original_sg_symbol_H-M      'C m'
_cod_database_code               7210632