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_7712164
_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             2023-01-10
_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                 95.810(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4587(15)
_cell_length_b                   11.0180(17)
_cell_length_c                   30.677(5)
_cell_measurement_reflns_used    7238
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.2850
_cell_measurement_theta_min      1.9530
_cell_volume                     3180.6(9)
_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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_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            20763
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        24.994
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         1.965
_exptl_absorpt_coefficient_mu    0.347
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.334
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.289
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         2714
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0421P)^2^+7.3011P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2145
_reflns_number_total             2714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03529d2.cif
_cod_data_source_block           nm_35b_100k
_cod_depositor_comments
'Adding full bibliography for 7712164--7712167.cif.'
_cod_database_code               7712164
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.897
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13B-C14A = C14A-C15B = C15B-C16B = C16B-C17B = C17B-C18B = C14A-C19B = C19B-
 C20A
 1.54 with sigma of 0.01
 C18B-C17B \\sim C18A-C17A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C16B) \\sim Ueq, Uanis(C15B) \\sim Ueq, Uanis(C14A) \\sim Ueq,
Uanis(C20A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
4. Rigid body (RIGU) restrains
 C13B, C14B, C15A, C16A, C17A, C18A, C19A, C20B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13A, C14A, C15B, C16B, C17B, C18B, C19B, C20A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C13A(0.6) H13A(0.6) H13B(0.6) C13B(0.4) H13C(0.4) H13D(0.4)
 C14A(0.6) H14A(0.6) C14B(0.4) H14B(0.4) C15A(0.4) H15A(0.4) H15B(0.4)
 C15B(0.6) H15C(0.6) H15D(0.6) C16A(0.4) H16A(0.4) H16B(0.4) C16B(0.6)
 H16C(0.6) H16D(0.6) C17A(0.4) H17A(0.4) H17B(0.4) C17B(0.6) H17C(0.6)
 H17D(0.6) C18A(0.4) H18A(0.4) H18B(0.4) H18C(0.4) C18B(0.6) H18D(0.6)
 H18E(0.6) H18F(0.6) C19A(0.4) H19A(0.4) H19B(0.4) C19B(0.6) H19C(0.6)
 H19D(0.6) C20A(0.6) H20A(0.6) H20B(0.6) H20C(0.6) C20B(0.4) H20D(0.4)
 H20E(0.4) H20F(0.4)
6.a Ternary CH refined with riding coordinates:
 C14A(H14A), C14B(H14B)
6.b Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C13B(H13C,H13D), C15A(H15A,H15B), C15B(H15C,H15D), C16A(H16A,
 H16B), C16B(H16C,H16D), C17A(H17A,H17B), C17B(H17C,H17D), C19A(H19A,H19B),
 C19B(H19C,H19D)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3A), C6(H6)
6.d Idealised Me refined as rotating group:
 C18A(H18A,H18B,H18C), C18B(H18D,H18E,H18F), C20A(H20A,H20B,H20C), C20B(H20D,
 H20E,H20F)
;
_olex2_submission_special_instructions 'No special instructions were received'