<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_7716403
_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 Gd N12 O12 P2, Cl, 1[CH3OH], 1[H2O]'
_chemical_formula_sum            'C14 H40 Cl Gd N12 O14 P2'
_chemical_formula_weight         855.22
_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                 96.725(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9642(6)
_cell_length_b                   13.9446(8)
_cell_length_c                   18.4472(12)
_cell_measurement_reflns_used    13861
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.9860
_cell_measurement_theta_min      2.5150
_cell_volume                     3312.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.00
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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    -35.00 -10.00   0.50   14.95    --    7.20 -28.00-121.00   50
  2  \w    -14.00  11.00   0.50   14.95    --   -7.60  28.00  41.00   50
  3  \w    -50.00 -25.00   0.50   14.95    --   -7.60 -28.00-121.00   50
  4  \w     51.00  96.00   0.50   14.95    --    7.20  77.00-150.00   90
  5  \w     50.00  90.00   0.50   14.95    --    7.20  77.00  90.00   80
  6  \w     68.00  97.00   0.50   14.95    --    7.20  77.00-120.00   58
  7  \w    -62.00   2.00   0.50   14.95    --   -7.60 -82.00 -90.00  128
  8  \w    -40.00 -14.00   0.50   14.95    --   -7.60 -82.00  60.00   52
  9  \w     10.00  35.00   0.50   14.95    --   -7.60 -82.00  60.00   50
 10  \w    -61.00   8.00   0.50   14.95    --   -7.60 -82.00 -30.00  138
 11  \w    -36.00  -9.00   0.50   14.95    --   -7.60 -82.00-150.00   54
 12  \w      8.00  36.00   0.50   14.95    --   -7.60 -82.00 -90.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33646
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.507
_exptl_absorpt_coefficient_mu    2.255
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (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    1.715
_exptl_crystal_description       block
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.922
_refine_diff_density_min         -1.337
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5770
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0328P)^2^+23.1763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1216
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4932
_reflns_number_total             5770
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00582a2.cif
_cod_data_source_block           gd
_cod_depositor_comments
'Adding full bibliography for 7716403--7716406.cif.'
_cod_database_code               7716403
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.674
_shelx_estimated_absorpt_t_min   0.637
_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
 O1-H1A
 0.85 with sigma of 0.01
 O4-H4
 0.85 with sigma of 0.01
 O2-H2
 0.85 with sigma of 0.01
 C1-H1A
 1.90228 with sigma of 0.02
 Gd1-H1A
 3.010024 with sigma of 0.02
 P1-H4
 1.942171 with sigma of 0.02
 Gd1-H4
 2.60943 with sigma of 0.02
 P2-H2
 1.941209 with sigma of 0.02
 Gd1-H2
 2.763712 with sigma of 0.02
3.a Riding coordinates:
 O1W(H1WA,H1WB)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N7(H7)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C13(H13A,H13B,H13C), C4(H4A,H4B,H4C), C12(H12A,H12B,H12C),
 C10(H10A,H10B,H10C), C1(H1B,H1C,H1D), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C),
 C5(H5A,H5B,H5C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 92 electrons were 
found in a volume of 520\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[CH3OH], 1[H2O] per formula unit 
which account for 112 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              84410
_shelx_fab_checksum              17896
_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
;