Facile room-temperature synthesis of layered transition metal phosphonates <i>via</i> hitherto unknown alkali metal <i>tert</i>-butyl phosphonates.
Kumar, Anuj; Ghatak, Aheli; Murugavel, Ramaswamy; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14399–14410; doi:10.1039/d4dt01668h

data_7716963
_publ_section_title
;
 Facile room-temperature synthesis of layered transition metal
 phosphonates <i>via</i> hitherto unknown alkali metal <i>tert</i>-butyl
 phosphonates.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14399
_journal_page_last               14410
_journal_paper_doi               10.1039/d4dt01668h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C4 H16 Li O6 P, H2 O'
_chemical_formula_sum            'C4 H18 Li O7 P'
_chemical_formula_weight         216.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-01-29
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2024-02-02 deposited with the CCDC.	2024-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                79.599(4)
_cell_angle_beta                 88.942(4)
_cell_angle_gamma                63.141(5)
_cell_formula_units_Z            2
_cell_length_a                   6.2774(3)
_cell_length_b                   6.5742(4)
_cell_length_c                   15.5423(8)
_cell_measurement_reflns_used    5115
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.5600
_cell_measurement_theta_min      2.6500
_cell_volume                     561.36(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -53.00  94.00   1.00    4.00    --    5.00  19.00 -90.00  147
  2  \w   -104.00  24.00   1.00    4.00    --  -14.30 -72.00  60.00  128
  3  \w   -104.00  24.00   1.00    4.00    --  -14.30 -72.00-180.00  128
  4  \w   -104.00  19.00   1.00    4.00    --  -14.30 -38.00 -90.00  123
  5  \w    -53.00  75.00   1.00    4.00    --  -14.30  72.00-120.00  128
  6  \w    -50.00  75.00   1.00    4.00    --  -14.30  57.00   0.00  125
  7  \w    -50.00  75.00   1.00    4.00    --  -14.30  57.00-150.00  125
  8  \w    -53.00 -15.00   1.00    4.00    --  -14.30  72.00  30.00   38
  9  \w    -53.00  75.00   1.00    4.00    --  -14.30  72.00  90.00  128
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0864606000
_diffrn_orient_matrix_UB_12      -0.0212878000
_diffrn_orient_matrix_UB_13      0.0336497000
_diffrn_orient_matrix_UB_21      0.0679488000
_diffrn_orient_matrix_UB_22      0.0315930000
_diffrn_orient_matrix_UB_23      -0.0316959000
_diffrn_orient_matrix_UB_31      -0.0635023000
_diffrn_orient_matrix_UB_32      0.1172212000
_diffrn_orient_matrix_UB_33      0.0052100000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0924
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12680
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         2.672
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       plate
_exptl_crystal_F_000             232
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1969
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1038P)^2^+0.2998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1661
_refine_ls_wR_factor_ref         0.1742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1700
_reflns_number_total             1969
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01668h2.cif
_cod_data_source_block           ak-251
_cod_database_code               7716963
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Li1 O5 P4'
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.929
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O7(H7A)
2.b Rotating group:
 O4(H4A,H4B), O5(H5A), O6(H6A,H6B)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4C,H4D,H4E)
2.d Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              9176
_shelx_hkl_checksum              85822
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.814
_oxdiff_exptl_absorpt_empirical_full_min 0.338