PCP and POCOP complexes of calcium
Messori, Alessandro; Potocnik, Marcel; Belazregue, Sara; Collins, Richard; Krämer, Tobias; Chadwick, F. Mark; Chemical Communications 61 (2025) 7827–7830; doi:10.1039/D5CC00872G

data_7134466
_publ_section_title
;
 PCP and POCOP complexes of calcium
;
_journal_issue                   43
_journal_name_full               'Chemical Communications'
_journal_page_first              7827
_journal_page_last               7830
_journal_paper_doi               10.1039/D5CC00872G
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C44 H78 Ca O4 P4'
_chemical_formula_sum            'C44 H78 Ca O4 P4'
_chemical_formula_weight         835.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-10
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-02-12 deposited with the CCDC.	2025-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.236(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.5873(7)
_cell_length_b                   11.5583(2)
_cell_length_c                   20.9001(7)
_cell_measurement_reflns_used    6584
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      73.5360
_cell_measurement_theta_min      4.2880
_cell_volume                     4972.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_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      5.00  98.00   1.00    7.50    --   42.36-125.00 120.00   93
  2  \w    -25.00  81.00   1.00    7.50    --   42.36 -19.00-120.00  106
  3  \w    -32.00  67.00   1.00    7.50    --   42.36 -38.00-180.00   99
  4  \w     46.00 115.00   1.00   30.00    --  105.75 -45.00-150.00   69
  5  \w    115.00 178.00   1.00   30.00    --  105.75  30.00 150.00   63
  6  \w     52.00 109.00   1.00   30.00    --  105.75 -95.00-120.00   57
  7  \w     33.00 109.00   1.00   30.00    --  105.75 -95.00   0.00   76
  8  \w     77.00 175.00   1.00   30.00    --  105.75  30.00 -90.00   98
  9  \w     30.00 106.00   1.00   30.00    --  105.75 -30.00 -30.00   76
 10  \w     34.00 115.00   1.00   30.00    --  105.75 -84.00 101.00   81
 11  \w     37.00 131.00   1.00   30.00    --  105.75 -45.00  90.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0628036000
_diffrn_orient_matrix_UB_12      0.0686562000
_diffrn_orient_matrix_UB_13      -0.0476556000
_diffrn_orient_matrix_UB_21      0.0201561000
_diffrn_orient_matrix_UB_22      0.0147667000
_diffrn_orient_matrix_UB_23      -0.0594279000
_diffrn_orient_matrix_UB_31      -0.0355054000
_diffrn_orient_matrix_UB_32      -0.1130518000
_diffrn_orient_matrix_UB_33      -0.0367400000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14032
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.739
_diffrn_reflns_theta_min         4.296
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.578
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85507
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense colourless'
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         4925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0537P)^2^+2.3143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1028
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4183
_reflns_number_total             4925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00872g2.cif
_cod_data_source_block           fmc2240
_cod_depositor_comments
'Adding full bibliography for 7134464--7134468.cif.'
_cod_database_code               7134466
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Ca1P4O4C44H78
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.627
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C4(H4)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C),
 C12(H12A,H12B,H12C), C22(H22A,H22B,H22C), C19(H19A,H19B,H19C), C13(H13A,H13B,
 H13C), C16(H16A,H16B,H16C), C21(H21A,H21B,H21C), C17(H17A,H17B,H17C), C18(H18A,
 H18B,H18C)
;
_shelx_res_checksum              56146
_shelx_hkl_checksum              20805
_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 1.185
_oxdiff_exptl_absorpt_empirical_full_min 0.840