Synthesis and Characterization of a Novel Cyclic Aluminophosphinate: Structure and Solid-State NMR Study
Thierry Azaïs; Laure Bonhomme-Coury; Jacqueline Vaissermann; Philippe Bertani; Jérôme Hirschinger; Jocelyne Maquet; Christian Bonhomme; Inorganic Chemistry 41 (2002) 981–988; doi:10.1021/ic010700k

data_4317544
_publ_contact_author
;
'Dr. C. Bonhomme, Laboratoire de Chimie de la Matiere Condensee, 
Universite Pierre et Marie Curie,
4 place Jussieu, 75252 Paris Cedex 05, France.'
,
;
_publ_contact_author_email       ' bonhomme@ccr.jussieu.fr '
_publ_contact_author_phone       ' 33 1 44 27 55 42 '
_publ_section_title
;
 Synthesis and Characterization of a Novel Cyclic Aluminophosphinate:
 Structure and Solid-State NMR Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              981
_journal_page_last               988
_journal_paper_doi               10.1021/ic010700k
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         ' C44 H92 Al2 P2 O12 4+, (Cl 1-)4'
_chemical_formula_sum            'C44 H92 Al2 Cl4 O12 P2'
_chemical_formula_weight         1070.9
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             00-05-09
_audit_creation_method           CRYSTALS
_cell_angle_alpha                90
_cell_angle_beta                 91.25(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.830(7)
_cell_length_b                   14.216(6)
_cell_length_c                   17.790(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    203
_cell_measurement_theta_max      14.2
_cell_measurement_theta_min      13.8
_cell_volume                     2991(2)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction
;
RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994)
;
_computing_molecular_graphics
;
CAMERON (Watkin, Prout & Pearce,  1996)
;
_computing_publication_material
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_computing_structure_refinement
;
CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996)
;
_diffrn_ambient_temperature      203
_diffrn_measurement_device       ' Enraf-nonius CAD4 '
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  ' graphite '
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.03
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5763
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1
_diffrn_standards_decay_%        17.90
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.33
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            ' none '
_exptl_crystal_density_diffrn    1.19
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             1133.89
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.36
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_obs   0.9693
_refine_ls_hydrogen_treatment
;
H atoms placed geometrically after each cycle,
one overall isotropic thermal parameter refined
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         2635
_refine_ls_R_factor_obs          0.0926
_refine_ls_shift/esd_max         1.172319
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
;
Chebychev polynomial (Carruthers & Watkin, 1979)
;
_refine_ls_wR_factor_obs         0.1146
_reflns_number_observed          2635
_reflns_number_total             5242
_reflns_observed_criterion       >3.00\s(I)
_cod_data_source_file            ic010700k.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_refine_ls_matrix_type' value ' full' changed to 'full'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value ' Direct_Methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value ' Geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        ' C44 H92 Cl4 Al2 P2 O12 '
_cod_database_code               4317544