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_7716964
_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 H10 K O4 P'
_chemical_formula_sum            'C4 H12 K O4 P'
_chemical_formula_weight         194.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-01-31
_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                90
_cell_angle_beta                 101.967(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6615(6)
_cell_length_b                   9.2070(4)
_cell_length_c                   7.0197(3)
_cell_measurement_reflns_used    5392
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.9120
_cell_measurement_theta_min      2.6670
_cell_volume                     863.76(7)
_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      100.0
_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    -48.00  75.00   1.00    8.00    --  -14.30  38.00 -30.00  123
  2  \w   -104.00  19.00   1.00    8.00    --  -14.30 -38.00 120.00  123
  3  \w    -48.00  75.00   1.00    8.00    --  -14.30  38.00-120.00  123
  4  \w   -104.00  24.00   1.00    8.00    --  -14.30 -72.00 -60.00  128
  5  \w    -53.00  75.00   1.00    8.00    --  -14.30  72.00   0.00  128
  6  \w   -104.00   0.00   1.00    8.00    --  -14.30 -57.00  60.00  104
  7  \w    -48.00  75.00   1.00    8.00    --  -14.30  38.00 120.00  123
;
_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      0.0291129000
_diffrn_orient_matrix_UB_12      -0.0628257000
_diffrn_orient_matrix_UB_13      0.0302977000
_diffrn_orient_matrix_UB_21      -0.0438330000
_diffrn_orient_matrix_UB_22      -0.0381141000
_diffrn_orient_matrix_UB_23      0.0096496000
_diffrn_orient_matrix_UB_31      -0.0068965000
_diffrn_orient_matrix_UB_32      -0.0230920000
_diffrn_orient_matrix_UB_33      -0.0982913000
_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  0.0647
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            14934
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.992
_diffrn_reflns_theta_max         24.992
_diffrn_reflns_theta_min         2.686
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85550
_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    1.493
_exptl_crystal_description       plate
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.374
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1520
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0815
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1377P)^2^+3.4259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2322
_refine_ls_wR_factor_ref         0.2350
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1435
_reflns_number_total             1520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01668h2.cif
_cod_data_source_block           ak-252
_cod_database_code               7716964
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'K1 C10 P2 O5'
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.869
_reflns_odcompleteness_completeness 99.95
_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
2. Restrained distances
 P1-O2
 1.508 with sigma of 0.02
3.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
3.b Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              32782
_shelx_hkl_checksum              30132
_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 1.796
_oxdiff_exptl_absorpt_empirical_full_min 0.618