<i>In situ</i> hydrolysis of a carbophosphazene ligand leads to one-dimensional lanthanide coordination polymers. Synthesis, structure and dynamic magnetic studies.
Ahmed, Naushad; Sahu, Prem Prakash; Chakraborty, Amit; Flores Gonzalez, Jessica; Ali, Junaid; Kalita, Pankaj; Pointillart, Fabrice; Singh, Saurabh Kumar; Chandrasekhar, Vadapalli; Dalton transactions (Cambridge, England : 2003) 53 (2024) 11563–11577; doi:10.1039/d4dt00582a

data_7716406
_publ_section_title
;
 <i>In situ</i> hydrolysis of a carbophosphazene ligand leads to
 one-dimensional lanthanide coordination polymers. Synthesis, structure
 and dynamic magnetic studies.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11563
_journal_page_last               11577
_journal_paper_doi               10.1039/d4dt00582a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C13 H34 Dy N12 O12 P2, Cl, C H4 O, 1[CH3OH]'
_chemical_formula_sum            'C15 H42 Cl Dy N12 O14 P2'
_chemical_formula_weight         874.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-28
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-02 deposited with the CCDC.	2024-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.668(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9512(3)
_cell_length_b                   13.8255(4)
_cell_length_c                   18.1765(6)
_cell_measurement_reflns_used    21048
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      29.0180
_cell_measurement_theta_min      2.9550
_cell_volume                     3225.52(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.890
_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    -17.00   8.00   0.50    6.59    --    7.20 -19.00 -61.00   50
  2  \w    -32.00  -7.00   0.50    6.59    --   -7.60 -19.00 -61.00   50
  3  \w    -32.00  -7.00   0.50    6.59    --   -7.60  19.00 106.00   50
  4  \w    -80.00  38.00   0.50    6.59    --    7.20 -57.00-120.00  236
  5  \w     51.00  83.00   0.50    6.59    --    7.20  77.00-120.00   64
  6  \w     71.00  97.00   0.50    6.59    --    7.20  77.00 -60.00   52
  7  \w    -62.00 -25.00   0.50    6.59    --    7.20 -82.00 150.00   74
  8  \w    -53.00  44.00   0.50    6.59    --    7.20 -82.00-150.00  194
  9  \w     -8.00  17.00   0.50    6.59    --    7.20 -82.00-120.00   50
 10  \w    -21.00   4.00   0.50    6.59    --   -7.60 -82.00  90.00   50
 11  \w    -62.00 -37.00   0.50    6.59    --   -7.60 -82.00  90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0180150000
_diffrn_orient_matrix_UB_12      0.0120773000
_diffrn_orient_matrix_UB_13      -0.0340216000
_diffrn_orient_matrix_UB_21      0.0513823000
_diffrn_orient_matrix_UB_22      0.0049829000
_diffrn_orient_matrix_UB_23      0.0187356000
_diffrn_orient_matrix_UB_31      0.0095389000
_diffrn_orient_matrix_UB_32      -0.0496083000
_diffrn_orient_matrix_UB_33      -0.0063948000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39612
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.036
_diffrn_reflns_theta_min         2.539
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.578
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_description       block
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         3.378
_refine_diff_density_min         -3.207
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         7673
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0322P)^2^+79.3250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1624
_refine_ls_wR_factor_ref         0.1671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6412
_reflns_number_total             7673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00582a2.cif
_cod_data_source_block           dy
_cod_depositor_comments
'Adding full bibliography for 7716403--7716406.cif.'
_cod_database_code               7716406
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O P Cl Dy '
_shelx_estimated_absorpt_t_max   0.640
_shelx_estimated_absorpt_t_min   0.565
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O4-H4
 0.87 with sigma of 0.01
 O2-H2
 0.87 with sigma of 0.01
 P1-H4
 1.956822 with sigma of 0.02
 Dy1-H4
 2.748928 with sigma of 0.02
 P2-H2
 1.959859 with sigma of 0.02
 Dy1-H2
 2.597923 with sigma of 0.02
3.a Riding coordinates:
 O1(H1), O1W(H1WA,H1WB), C1(H1A,H1B,H1C)
3.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C1S(H1SA,H1SB,H1SC)
3.d Idealised tetrahedral OH refined as rotating group:
 O1S(H1S)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 68 electrons were 
found in a volume of 216\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[CH3OH] per formula unit 
which account for 72 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              10456
_shelx_fab_checksum              3479
_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 1.270
_oxdiff_exptl_absorpt_empirical_full_min 0.830