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_7134468
_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         'C28 H57 Ca N O2 P2 Si2'
_chemical_formula_sum            'C28 H57 Ca N O2 P2 Si2'
_chemical_formula_weight         597.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.8629(2)
_cell_length_b                   19.3315(2)
_cell_length_c                   25.3975(3)
_cell_measurement_reflns_used    6740
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      73.5160
_cell_measurement_theta_min      4.1200
_cell_volume                     7297.26(15)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4115
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.966
_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   -117.00 -82.00   1.00   25.00    --  -42.36 -38.00   0.00   35
  2  \w    -44.00 -18.00   1.00   25.00    --  -42.36 -38.00   0.00   26
  3  \w     90.00 178.00   1.00  100.00    --  105.75  30.00 120.00   88
  4  \w    -67.00  29.00   1.00   25.00    --  -42.36  38.00-180.00   96
  5  \w     87.00 166.00   1.00  100.00    --  105.75  45.00-150.00   79
  6  \w     33.00 106.00   1.00  100.00    --  105.75 -45.00 120.00   73
;
_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      0.0576640000
_diffrn_orient_matrix_UB_12      0.0299551000
_diffrn_orient_matrix_UB_13      0.0449459000
_diffrn_orient_matrix_UB_21      0.0070701000
_diffrn_orient_matrix_UB_22      0.0691521000
_diffrn_orient_matrix_UB_23      -0.0298110000
_diffrn_orient_matrix_UB_31      -0.0859152000
_diffrn_orient_matrix_UB_32      0.0258625000
_diffrn_orient_matrix_UB_33      0.0277034000
_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  0.0361
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17163
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.745
_diffrn_reflns_theta_min         3.480
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.106
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72877
_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 light colourless'
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         7127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0552P)^2^+2.6880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1203
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5581
_reflns_number_total             7127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00872g2.cif
_cod_data_source_block           fmc2223
_cod_depositor_comments
'Adding full bibliography for 7134464--7134468.cif.'
_cod_database_code               7134468
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ca1 P2 O2 Si2 N1 C28 H57'
_shelx_estimated_absorpt_t_max   0.746
_shelx_estimated_absorpt_t_min   0.456
_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:
 C5(H5), C4(H4), C3(H3)
2.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C12(H12A,H12B,H12C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C),
 C28(H28A,H28B,H28C), C24(H24A,H24B,H24C), C14(H14A,H14B,H14C), C13(H13A,H13B,
 H13C), C10(H10A,H10B,H10C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C20(H20A,
 H20B,H20C), C18(H18A,H18B,H18C), C16(H16A,H16B,H16C), C22(H22A,H22B,H22C),
 C17(H17A,H17B,H17C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              49442
_shelx_hkl_checksum              66185
_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 1.311
_oxdiff_exptl_absorpt_empirical_full_min 0.839