A rigid calcium 2-ethylhexylphosphate one-dimensional polymer: synthesis, structure, thermal behaviour and decomposition chemistry.
Matharoo, Navneet; Walawalkar, Mrinalini G.; Murugavel, Ramaswamy; Dalton transactions (Cambridge, England : 2003) 52 (2023) 2412–2423; doi:10.1039/d2dt03529d

data_7712166
_publ_section_title
;
 A rigid calcium 2-ethylhexylphosphate one-dimensional polymer: synthesis,
 structure, thermal behaviour and decomposition chemistry.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2412
_journal_page_last               2423
_journal_paper_doi               10.1039/d2dt03529d
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C28 H44 Ca N2 O8 P2'
_chemical_formula_sum            'C28 H44 Ca N2 O8 P2'
_chemical_formula_weight         638.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-01-08
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-11 deposited with the CCDC.	2023-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.050(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4853(3)
_cell_length_b                   11.0551(3)
_cell_length_c                   30.9403(12)
_cell_measurement_reflns_used    3853
_cell_measurement_temperature    233.15
_cell_measurement_theta_max      21.8870
_cell_measurement_theta_min      1.9510
_cell_volume                     3226.36(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      233.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            31460
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.957
_exptl_absorpt_coefficient_mu    0.342
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.45171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.441
_exptl_crystal_size_mid          0.277
_exptl_crystal_size_min          0.011
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         2842
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0699P)^2^+2.0291P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2028
_reflns_number_total             2842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03529d2.cif
_cod_data_source_block           nm_ehp_233k
_cod_depositor_comments
'Adding full bibliography for 7712164--7712167.cif.'
_cod_database_code               7712166
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.864
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C14A-C15A \\sim C14B-C15B
 with sigma of 0.02
 C14A-C19A \\sim C14B-C19B
 with sigma of 0.02
 C19A-C20A \\sim C19B-C20B
 with sigma of 0.02
 C15A-C19A \\sim C15B-C19B
 with sigma of 0.04
 C15A-C16A \\sim C15B-C16B
 with sigma of 0.02
 C16A-C17A \\sim C16B-C17B
 with sigma of 0.02
 C17A-C18A \\sim C17B-C18B
 with sigma of 0.02
 O4-C14A \\sim O4-C14B
 with sigma of 0.04
 C14A-C16A \\sim C14B-C16B
 with sigma of 0.04
 C14A-C20A \\sim C14B-C20B
 with sigma of 0.04
 C15A-C17A \\sim C15B-C17B
 with sigma of 0.04
 C16A-C18A \\sim C16B-C18B
 with sigma of 0.04
 C16B-C15B \\sim C17B-C16B \\sim C18B-C17B \\sim C15B-C14B \\sim C15A-C14A
\\sim C16A-C15A \\sim C17A-
 C16A \\sim C18A-C17A
 with sigma of 0.0001
3. Uiso/Uaniso restraints and constraints
C19A \\sim C19B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C17B \\sim C17A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
C20B \\sim C20A: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002 within 2A
4. Rigid body (RIGU) restrains
 C13A, C17A, C19A, C14A, C18A, C15A, C20A, C16A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17B, C19B, C14B, C18B, C15B, C20B, C16B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H13C)=Sof(H13D)=Sof(C14B)=Sof(H14B)=Sof(C15B)=Sof(H15C)=Sof(H15D)=
 Sof(C16B)=Sof(H16C)=Sof(H16D)=Sof(C17B)=Sof(H17C)=Sof(H17D)=Sof(C18B)=
 Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19B)=Sof(H19C)=Sof(H19D)=Sof(C20B)=
 Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(1)
 Sof(H13A)=Sof(H13B)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(H15B)=
 Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(C17A)=Sof(H17A)=Sof(H17B)=Sof(C18A)=
 Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(C20A)=
 Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(1)
6.a Riding coordinates:
 C18A(H18A,H18B,H18C), C18B(H18D,H18E,H18F)
6.b Ternary CH refined with riding coordinates:
 C14A(H14A), C14B(H14B)
6.c Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C13A(H13C,H13D), C15A(H15A,H15B), C16A(H16A,H16B), C17A(H17A,
 H17B), C19A(H19A,H19B), C15B(H15C,H15D), C16B(H16C,H16D), C17B(H17C,H17D),
 C19B(H19C,H19D)
6.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3A), C6(H6)
6.e Idealised Me refined as rotating group:
 C20A(H20A,H20B,H20C), C20B(H20D,H20E,H20F)
6.f Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'