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_7716965
_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 H11 Na2 O7 P'
_chemical_formula_sum            'C4 H17 Na2 O7 P'
_chemical_formula_weight         254.12
_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   mixed
_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                 104.188(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5571(5)
_cell_length_b                   6.79238(16)
_cell_length_c                   13.4207(3)
_cell_measurement_reflns_used    4288
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.0480
_cell_measurement_theta_min      2.8650
_cell_volume                     1286.53(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      100
_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   -104.00  21.00   1.00   10.00    --  -14.30 -57.00-180.00  125
  2  \w    -48.00  75.00   1.00   10.00    --  -14.30  38.00  90.00  123
  3  \w   -104.00  21.00   1.00   10.00    --  -14.30 -57.00 -90.00  125
  4  \w    -50.00  75.00   1.00   10.00    --  -14.30  57.00-150.00  125
  5  \w   -104.00  21.00   1.00   10.00    --  -14.30 -57.00  60.00  125
  6  \w    -53.00  73.00   1.00   10.00    --  -14.30  72.00   0.00  126
  7  \w    -50.00  75.00   1.00   10.00    --  -14.30  57.00 -90.00  125
;
_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      -0.0401327000
_diffrn_orient_matrix_UB_12      -0.0625222000
_diffrn_orient_matrix_UB_13      -0.0141136000
_diffrn_orient_matrix_UB_21      -0.0298987000
_diffrn_orient_matrix_UB_22      0.0801350000
_diffrn_orient_matrix_UB_23      0.0046633000
_diffrn_orient_matrix_UB_31      -0.0046684000
_diffrn_orient_matrix_UB_32      0.0239619000
_diffrn_orient_matrix_UB_33      -0.0524446000
_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  0.0771
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22368
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.887
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.288
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40217
_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    1.312
_exptl_crystal_description       plate
_exptl_crystal_F_000             536
_exptl_crystal_preparation       0
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2250
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0953
_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^)+(0.1414P)^2^+3.5181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2483
_refine_ls_wR_factor_ref         0.2563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2039
_reflns_number_total             2250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01668h2.cif
_cod_data_source_block           ak-242
_cod_original_cell_volume        1286.53(7)
_cod_database_code               7716965
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C12H12O4PNa
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.802
_reflns_odcompleteness_completeness 99.93
_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,H) groups
2. Restrained distances
 O5-H5A
 0.88 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)
;
_shelx_res_checksum              25790
_shelx_hkl_checksum              67950
_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 1.919
_oxdiff_exptl_absorpt_empirical_full_min 0.562